Method for preparing diiodosilane
A safe and efficient method for producing diiodosilane using stable compounds in controlled reactions with iodine in mixed solvents addresses the safety and efficiency issues of conventional methods, achieving high-purity diiodosilane through filtration and distillation.
Patent Information
- Application Number
- JP2025061857
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-07-16
- Filing Date
- 2025-04-03
- Publication Date
- 2025-10-17
AI Technical Summary
Conventional methods for producing diiodosilane face challenges such as the use of flammable and toxic raw materials, high production costs, explosion risks, and reduced yields due to intense heat generation, making the process unsafe and inefficient.
A method involving the reaction of a compound represented by Chemical Formula 1 with iodine in a mixed solvent of an ester-based organic solvent and a halogenated hydrocarbon-based solvent at controlled temperatures, followed by filtration and distillation to produce high-purity diiodosilane.
The method ensures process safety and productivity by using stable, easy-to-handle materials, reduces heat generation, and allows for the safe removal of by-products, resulting in high-purity diiodosilane production.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to a method for producing diiodosilane. [Background technology]
[0002] Diiodosilane (SiH2I2) is a compound that plays an important role in the fields of semiconductor manufacturing and new material development, and demand for this compound is increasing with the continuous development of the semiconductor industry.
[0003] In conventional technology, the main synthesis method for diiodosilane is to replace the Si-Cl bond in dichlorosilane (SiH2Cl2) with Si-I using expensive lithium iodide, etc. However, the raw material dichlorosilane is a flammable gas at room temperature and reacts with moisture to produce toxic hydrogen chloride gas, so special care is required during storage.
[0004] Meanwhile, a synthesis method for producing diiodosilane by reacting phenylsilane with iodine has been proposed, but this method has problems such as the raw material phenylsilane being an expensive material, resulting in reduced productivity, explosion upon contact with moisture, and difficulty in storage due to its high moisture absorption rate. Furthermore, the reaction process generates intense heat, which can lead to explosions, making the process highly dangerous, resulting in reduced yields, and producing benzene, a carcinogenic by-product. [Prior art documents] [Patent documents]
[0005] [Patent Document 1] US Patent Application Publication No. 2016 / 0264426 Summary of the Invention [Problem to be solved by the invention]
[0006] An embodiment of the present invention is to provide a production method that can ensure process safety and productivity while also producing high-purity diiodosilane. [Means for solving the problem]
[0007] A method for producing diiodosilane according to one embodiment of the present invention may include a step of reacting a compound represented by the following Chemical Formula 1 with iodine (I2) to produce diiodosilane (SiH2I2). [ka] (In chemical formula 1, R is hydrogen or -NR 1 R 2 and R 1 and R 2 are each independently hydrogen or C1-C10 alkyl; A is -NR 3 R 4 -OR 5 and R 3 ~R 5 are each independently hydrogen, C1-C10 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 and R 3 and R 4 may be linked by a C3-C7 alkylene or a C2-C7 heteroalkylene to form a heterocycle; The heterocycle and R 3 ~R 5 The alkyl is -SiR 14 R 15 R 16 or -OSiR 17 R 18 R 19 may be substituted with R 11 ~R 19 are each independently hydrogen or C1-C10 alkyl.
[0008] The compound represented by Chemical Formula 1 may be represented by Chemical Formula 2 or Chemical Formula 3 below. [ka] [ka] (In Chemical Formulas 2 and 3, A, R 1 , and R 2 is as defined in Chemical Formula 1 above, R 21 and R 22 are each independently hydrogen, C1-C10 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 and R 11 ~R 13 are each independently hydrogen or C1-C10 alkyl.
[0009] R 1 , R 2 , R 21 , and R 22 may each independently be hydrogen or C1-C4 alkyl.
[0010] R 5 is C1-C10 alkyl or -L 1 -OSiR 17 R 18 R 19 and L 1 is C1-C10 alkylene, and R 17 ~R 19 may each independently be hydrogen or C1-C10 alkyl.
[0011] The compound represented by Chemical Formula 2 may be represented by Chemical Formula 4 or Chemical Formula 5 below. [ka] [ka] (In Chemical Formulas 4 and 5, R 31 and R 32 are each independently hydrogen, C1-C7 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 Or R 31 and R 32 is C3-C7 alkylene or *-L 2 -X 1 -L 3 may be linked by -* to form a heterocycle, L 2 and L 3 are each independently C1-C3 alkylene; X 1 is a single bond, -O-, or -NR 35 and R 35 is hydrogen or -SiR 14 R 15 R 16 and R 33 is C1-C4 alkyl, R 34 is C1-C4 alkyl or -OSiR 17 R 18 R 19 and R 11 ~R 19 are each independently hydrogen or C1-C7 alkyl.
[0012] The compound represented by Chemical Formula 1 may be selected from the following structures: [ka]
[0013] The method for producing diiodosilane according to one embodiment may further include a step of reacting hydrogen iodide (HI).
[0014] The reaction may be carried out in a mixed solvent containing an ester-based organic solvent and a halogenated hydrocarbon-based organic solvent.
[0015] The reaction may be carried out at a temperature of 10 to 40°C.
[0016] The method for producing diiodosilane according to one embodiment may further include the step of filtering the iodate salt after the reaction and purifying it by distillation. [Effects of the Invention]
[0017] The production method according to one embodiment is advantageous in terms of commercialization because it uses starting materials that are liquid and stable at room temperature, making them easy to store and handle.
[0018] The production method according to one embodiment does not generate excessive heat during the reaction, making the process safer and reducing the energy required for cooling. Furthermore, the reaction by-product, iodate, can be safely and easily removed by filtration, allowing high-purity diiodosilane to be obtained through a simple process. DETAILED DESCRIPTION OF THE INVENTION
[0019] Unless otherwise defined herein, all technical and scientific terms have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terms used in the description of this specification are merely for the purpose of effectively describing specific embodiments and are not intended to limit the present invention.
[0020] As used herein, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly dictates otherwise.
[0021] Throughout this specification, "comprise," "equipped," "contain," or "have" an element means not to the exclusion of other elements, but may further include other elements, and does not exclude additional, unrecited elements, materials, or steps, unless otherwise specified to the contrary.
[0022] Numerical ranges used herein include lower and upper limits, all values within the range, increments logically derived from the form and width of the defined range, all doubly limited values, and all possible combinations of upper and lower limits of numerical ranges limited in different forms. Unless otherwise defined herein, values outside the numerical ranges that may occur due to experimental error or rounding of values are also included in the defined numerical range.
[0023] As used herein, the term "alkyl" refers to an organic radical derived from an aliphatic hydrocarbon by the removal of one hydrogen and can include both straight and branched chains. Examples include, but are not limited to, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, t-butyl, pentyl, hexyl, ethylhexyl, and the like.
[0024] As used herein, the term "alkylene" refers to a divalent organic radical derived from an aliphatic hydrocarbon by the removal of two hydrogens, and can include both straight and branched chains. Examples include, but are not limited to, methylene, ethylene, propylene, isopropylene, butylene, isobutylene, t-butylene, pentylene, hexylene, octylene, nonylene, and the like.
[0025] As used herein, the term "heteroalkylene" refers to an alkylene containing one or more heteroatoms selected from B, N, O, S, P(=O), Si, and P, where alkylene is as defined above.
[0026] The term "aryl" as used herein refers to an organic radical derived from an aromatic hydrocarbon by removal of one hydrogen atom, and includes single or fused ring systems suitably containing 4 to 7, preferably 5 or 6, ring atoms in each ring, and may also include multiple aryls linked by single bonds. Examples include, but are not limited to, phenyl, naphthyl, biphenyl, fluorenyl, terphenyl, etc.
[0027] Unless otherwise defined herein, "about" may contemplate a value within 30%, 25%, 20%, 15%, 10%, or 5% of the stated value.
[0028] The present disclosure will now be described in detail, but by way of example only, and the present disclosure is not limited to the specific embodiments illustratively described.
[0029] One aspect of the present invention provides a production method that can ensure process safety and productivity while also producing high-purity diiodosilane.
[0030] Specifically, a method for producing diiodosilane according to one embodiment may include a step of reacting a compound represented by the following Chemical Formula 1 with iodine (I2) to produce diiodosilane (SiH2I2). [ka] (In chemical formula 1, R is hydrogen or -NR 1 R 2 and R 1 and R 2 are each independently hydrogen or C1-C10 alkyl; A is -NR 3 R 4 -OR 5 and R 3 ~R 5 are each independently hydrogen, C1-C10 alkyl, C6-C12 aryl, or -SiR11 R 12 R 13 and R 3 and R 4 may be linked by a C3-C7 alkylene or a C2-C7 heteroalkylene to form a heterocycle; The heterocycle and R 3 ~R 5 The alkyl is -SiR 14 R 15 R 16 or -OSiR 17 R 18 R 19 may be substituted with R 11 ~R 19 are each independently hydrogen or C1-C10 alkyl.
[0031] As an example, R 1 and R 2 may each independently be hydrogen or C1-C7 alkyl, specifically hydrogen or C1-C4 alkyl.
[0032] As an example, R 3 and R 4 are each independently hydrogen, C1-C7 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 It may be.
[0033] As an example, R 3 and R 4 are each independently hydrogen, C1-C4 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 It may be.
[0034] As an example, R 11 ~R 13 may each independently be hydrogen or C1-C7 alkyl, may be hydrogen or C1-C4 alkyl, and specifically may be hydrogen or methyl.
[0035] As an example, R 3 and R 4 is C3-C7 alkylene or *-L 2 -X 1 -L 3 -* to form a heterocycle, and L 2 and L 3 are each independently C1-C3 alkylene; X 1 is a single bond, -O-, or -NR 35 and R 35 is hydrogen or -SiR 14 R 15 R 16 and R 14 ~R 16 may each independently be hydrogen or C1-C7 alkyl.
[0036] As an example, R 14 ~R 16 may each independently be hydrogen or C1-C4 alkyl, specifically hydrogen or methyl.
[0037] The compound represented by Chemical Formula 1 may be represented by Chemical Formula 2 or Chemical Formula 3 below.
[0038] [ka] [ka] (In Chemical Formulas 2 and 3, A, R 1 , and R 2 is as defined in Chemical Formula 1, R 21 and R 22 are each independently hydrogen, C1-C10 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 and R 11 ~R 13are each independently hydrogen or C1-C10 alkyl.
[0039] As an example, R 21 and R 22 are each independently hydrogen, C1-C7 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 Specifically, R 21 and R 22 are each independently hydrogen, C1-C4 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 It may be.
[0040] As an example, R 1 , R 2 , R 21 , and R 22 may each independently be hydrogen or C1-C4 alkyl.
[0041] As an example, R 1 and R 21 are the same as each other and may be hydrogen or C1-C4 alkyl.
[0042] As an example, R 2 and R 22 are the same as each other and may be hydrogen or C1-C4 alkyl.
[0043] As an example, R 5 is C1-C10 alkyl or -L 1 -OSiR 17 R 18 R 19 and L 1 is C1-C10 alkylene, and R 17 ~R 19 may each independently be hydrogen or C1-C10 alkyl.
[0044] As an example, R 5 is a branched C3-C10 alkyl or -L1 -OSiR 17 R 18 R 19 and L 1 is a branched C alkylene, and R 17 ~R 19 may each independently be hydrogen or C1-C10 alkyl.
[0045] As an example, R 5 is a branched C3-C7 alkyl or -L 1 -OSiR 17 R 18 R 19 and L 1 is a branched C alkylene; R 17 ~R 19 may each independently be hydrogen or C1-C7 alkyl.
[0046] As an example, R 17 ~R 19 may each independently be hydrogen or C1-C4 alkyl, specifically hydrogen or methyl.
[0047] The compound represented by Chemical Formula 2 may be represented by Chemical Formula 4 or Chemical Formula 5 below. [ka] [ka] (In Chemical Formulas 4 and 5, R 31 and R 32 are each independently hydrogen, C1-C7 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 Or R 31 and R 32 is C3-C7 alkylene or *-L 2 -X 1 -L 3may be linked by -* to form a heterocycle, L 2 and L 3 are each independently C1-C3 alkylene; X 1 is a single bond, -O-, or -NR 35 and R 35 is hydrogen or -SiR 14 R 15 R 16 and R 33 is C1-C4 alkyl, R 34 is C1-C4 alkyl or -OSiR 17 R 18 R 19 and R 11 ~R 19 are each independently hydrogen or C1-C7 alkyl.
[0048] As an example, R 31 and R 32 are each independently hydrogen, C1-C4 alkyl, C6-C12 aryl, or -SiR 11 R 12 R 13 It may be.
[0049] Specifically, the compound represented by Chemical Formula 1 may be selected from the following structures, but is not limited thereto. [ka]
[0050] In one embodiment of the production method, the reaction may be carried out in an organic solvent. The organic solvent is not particularly limited as long as it can easily dissolve the starting materials, and examples include alcoholic solvents such as methanol, ethanol, n-propanol, isopropanol, n-butanol, and isobutanol; ester solvents such as ethyl acetate, butyl acetate, and 3-methoxy-3-methylbutyl acetate; ether solvents such as dimethyl ether and dibutyl ether; ketone solvents such as acetone, methyl ethyl ketone, methyl isobutyl ketone, and acetophenone; and halogenated hydrocarbon solvents such as dichloromethane, dichloroethane, chloroform, carbon tetrachloride, trichloroethylene, and perfluoropropane.
[0051] Specifically, the reaction may be carried out in a mixed solvent containing an ester organic solvent and a halogenated hydrocarbon organic solvent, wherein the mixed solvent contains the ester organic solvent and the halogenated hydrocarbon organic solvent in a molar ratio of 1:10-100, 1:20-100, 1:20-70, 1:30-70, or 1:40-70.
[0052] The reaction may be carried out at a temperature of 10 to 40°C or 20 to 40°C for 10 to 40 hours, 10 to 30 hours, or 20 to 30 hours.
[0053] The method for producing diiodosilane according to one embodiment may further include the step of filtering the iodate salt after the reaction and purifying it by distillation.
[0054] Specifically, a method for producing diiodosilane according to one embodiment may include the steps of adding iodine to a halogenated hydrocarbon organic solvent, adding a compound represented by Chemical Formula 1 and an ester organic solvent to react with each other, and filtering the iodate salt produced after the reaction and purifying it by distillation.
[0055] The production method according to one embodiment may further include a step of reacting hydrogen iodide (HI). In this case, the method may include a step of adding iodine to a halogenated hydrocarbon organic solvent, a step of adding the compound represented by Chemical Formula 1 and an ester organic solvent to react with each other, a step of bubbling hydrogen iodide and then further stirring the mixture, and a step of filtering the iodate produced by the reaction and purifying it by distillation.
[0056] The above-mentioned implementation will be described in more detail below with reference to examples, which are for illustrative purposes only and are not intended to limit the scope of the invention.
[0057] <Synthesis of diiodosilane> [Example 1] [ka] Under an anhydrous and inert atmosphere, a flame-dried 100 mL flask was charged with 1028 g (4.05 mol) of iodine (I2) and 464 mL (5.79 mol) of chloroform. A mixture of 253 g (1.93 mol) of diisopropylaminosilane and 9.5 mL (0.1 mol) of ethyl acetate was slowly added at an internal temperature between 5 and 25 °C, and the mixture was stirred at room temperature for 24 hours. After the reaction was complete, the reaction mixture was filtered to remove diisopropylamine hydroiodide, and the solvent was removed from the filtrate under reduced pressure. The mixture was purified by distillation at 38-40 °C and 8-9 torr, producing 176 g of diiodosilane (32.13% yield, 98.72% NMR purity). 1 H NMR (C6D6): 3.57 ppm (s, 2H) 29 Si NMR (C6D6): -98.8 ppm (s, 1Si)
[0058] [Example 2] [ka] Under an anhydrous and inert atmosphere, a flame-dried 100 mL flask was charged with 34.8 g (0.14 mol) of iodine and 23.4 g (0.20 mol) of chloroform, and a mixture of 10 g (0.07 mol) of disilylphenylamine and 0.29 g (0.003 mol) of ethyl acetate was slowly added at an internal temperature between 5 and 30 °C. The mixture was then stirred at room temperature for 24 hours. After the reaction was complete, the reaction mixture was filtered to remove aniline hydroiodide, and the solvent was removed from the filtrate under reduced pressure. The mixture was purified by distillation at 38-40 °C and 8-9 torr to produce 11.9 g of diiodosilane (32% yield, 98.13% NMR purity). 1 H NMR (C6D6): 3.57 ppm (s, 2H) 29 Si NMR (C6D6): -100.1 ppm (s, 1Si)
[0059] [Example 3] [ka] Under an anhydrous and inert atmosphere, a flame-dried 100 mL flask was charged with 40.3 g (0.16 mol) of iodine and 27.1 g (0.23 mol) of chloroform, and then a mixture of 10 g (0.08 mol) of 1,3-disilylimidazolidine and 0.33 g (0.004 mol) of ethyl acetate was slowly added at an internal temperature of 5-30°C. The mixture was then stirred at room temperature for 24 hours. After the reaction was complete, the reaction mixture was filtered to remove imidazolidine dihydroiodide, and the solvent was removed from the filtrate under reduced pressure. The mixture was purified by distillation at 38-40°C and 8-9 torr to produce 5.4 g (25% yield) of diiodosilane. 1 H NMR (C6D6): 3.57 ppm (s, 2H) 29 Si NMR (C6D6): -98.8 ppm (s, 1Si)
[0060] [Example 4] [ka] Under an anhydrous and inert atmosphere, a flame-dried 100 mL flask was charged with 30.6 g (0.12 mol) of iodine and 20.5 g (0.17 mol) of chloroform, and a mixture of 10 g (0.06 mol) of bis-diethylaminosilane and 0.25 g (0.003 mol) of ethyl acetate was slowly added at an internal temperature of 5–25°C. The mixture was then stirred at room temperature for 24 hours. After the reaction was complete, the reaction mixture was filtered to remove diethylamine hydroiodide, and the solvent was removed from the filtrate under reduced pressure. The mixture was purified by distillation at 30–35°C and 3–5 torr to produce 4.6 g (28% yield) of diiodosilane. 1 H NMR (C6D6): 3.57 ppm (s, 2H) 29 Si NMR (C6D6): -98.8 ppm (s, 1Si)
[0061] [Example 5] [ka] Under an anhydrous and inert atmosphere, a flame-dried 100 mL flask was charged with 30.6 g (0.12 mol) of diiodine and 20.5 g (0.17 mol) of chloroform, and a mixture of 10 g (0.06 mol) of bis-diethylaminosilane and 0.25 g (0.003 mol) of ethyl acetate was slowly added at an internal temperature between 15 and 30 °C. The mixture was then stirred at room temperature for 12 hours. After cooling to 0 °C, 7.3 g (0.06 mol) of hydrogen iodide (HI) was bubbled into the flask and the mixture was stirred at room temperature for 2 hours. After the reaction was complete, the reaction mixture was filtered to remove diethylamine hydroiodide, and the solvent was removed from the resulting filtrate under reduced pressure. The mixture was purified by distillation at 30 to 35°C and 3 to 5 torr to produce 4.6 g of diiodosilane (yield 28.8%). 1 H NMR (C6D6): 3.50ppm (s, 2H) 29 Si NMR (C6D6): -98.8 ppm (s, 1Si)
[0062] [Example 6] [ka] Under an anhydrous and inert atmosphere, a flame-dried 100 mL flask was charged with 30.6 g (0.12 mol) of diiodine and 20.5 g (0.17 mol) of chloroform, and a mixture of 10 g (0.06 mol) of bis(tertbutylamino)silane and 0.25 g (0.003 mol) of ethyl acetate was slowly added at an internal temperature between 5 and 25 °C. The mixture was then stirred at room temperature for 24 hours. After the reaction was complete, the reaction mixture was filtered to remove tertbutylamine hydroiodide, and the solvent was removed from the filtrate under reduced pressure. The mixture was purified by distillation at 30-35 °C and 3-5 torr to produce 3.7 g (23% yield) of diiodosilane. 1 H NMR (C6D6): 3.57 ppm (s, 2H) 29 Si NMR (C6D6): -98.8 ppm (s, 1Si)
[0063] [Example 7] [ka] Under an anhydrous and inert atmosphere, a flame-dried 100 mL flask was charged with 30.6 g (0.12 mol) of diiodine and 20.5 g (0.17 mol) of chloroform, and a mixture of 10 g (0.06 mol) of bis(tertbutylamino)silane and 0.25 g (0.003 mol) of ethyl acetate was slowly added at an internal temperature between 15 and 30 °C. The mixture was then stirred at room temperature for 12 hours. After cooling to 0 °C, 7.3 g (0.06 mol) of hydrogen iodide (HI) was bubbled into the flask and the mixture was stirred at room temperature for 2 hours. After the reaction was complete, the reaction mixture was filtered to remove tertbutylamine hydroiodide, and the solvent was removed from the resulting filtrate under reduced pressure. The mixture was purified by distillation at 30 to 35° C. and 3 to 5 torr to produce 3.7 g (yield 23%) of diiodosilane. 1 H NMR (C6D6): 3.50ppm (s, 2H) 29 Si NMR (C6D6): -98.8 ppm (s, 1Si)
[0064] As described above, the present invention has been described using specific and limited examples and comparative examples. However, these are merely provided for a more general understanding of the present invention, and the present invention is not limited to the above examples. Those skilled in the art will appreciate that various modifications and variations can be made from such descriptions.
[0065] Therefore, the spirit of the present invention should not be limited to the above-described embodiments, and it can be said that not only the scope of the attached claims, but also anything equivalent to the scope of the claims or any equivalent modifications thereof, all fall within the scope of the spirit of the present invention.
Claims
1. A method for producing diiodosilane, comprising the step of reacting a compound represented by the following chemical formula 1 with iodine (I 2 ), to produce diiodosilane (SiH 2 I 2 ). 【Chemical 1】 (In chemical formula 1, R is hydrogen or —NR 1 R 2 and R 1 and R 2 are each independently hydrogen or C1-C10 alkyl; A is -NR 3 R 4 or -OR 5 and R 3 ~R 5 are each independently hydrogen, C1-C10 alkyl, C6-C12 aryl, or —SiR 11 R 12 R 13 and the R 3 and R 4 may be linked by a C3-C7 alkylene or a C2-C7 heteroalkylene to form a heterocycle; The heterocycle and R 3 ~R 5 The alkyl is —SiR 14 R 15 R 16 or -OSiR 17 R 18 R 19 may be substituted with R 11 ~R 19 are each independently hydrogen or C1-C10 alkyl.
2. The method for producing diiodosilane according to claim 1, wherein the compound represented by Chemical Formula 1 is represented by the following Chemical Formula 2 or Chemical Formula 3: 【Chemistry 2】 【Chemistry 3】 (In Chemical Formulas 2 and 3, A, R 1 , and R 2 is as defined in claim 1, R 21 and R 22 are each independently hydrogen, C1-C10 alkyl, C6-C12 aryl, or —SiR 11 R 12 R 13 and R 11 ~R 13 are each independently hydrogen or C1-C10 alkyl.
3. R 1 , R 2 , R 21 , and R 22 are each independently hydrogen or C1-C4 alkyl.
4. R 5 is C1-C10 alkyl or -L 1 -OSiR 17 R 18 R 19 and L 1 is a C1-C10 alkylene; R 17 ~R 19 are each independently hydrogen or C1-C10 alkyl.
5. The method for producing diiodosilane according to claim 2, wherein the compound represented by Chemical Formula 2 is represented by the following Chemical Formula 4 or Chemical Formula 5: 【Chemistry 4】 【Chemistry 5】 (In Chemical Formulas 4 and 5, R 31 and R 32 are each independently hydrogen, C1-C7 alkyl, C6-C12 aryl, or —SiR 11 R 12 R 13 Or The R 31 and R 32 is C3-C7 alkylene or *-L 2 -X 1 -L 3 may be linked by -* to form a heterocycle, L 2 and L 3 are each independently C1-C3 alkylene; X 1 represents a single bond, —O—, or —NR 35 and R 35 is hydrogen or —SiR 14 R 15 R 16 and R 33 is C1-C4 alkyl, R 34 is C1-C4 alkyl or —OSiR 17 R 18 R 19 and R 11 ~R 19 are each independently hydrogen or C1-C7 alkyl.
6. 2. The method for producing diiodosilane according to claim 1, wherein the compound represented by Chemical Formula 1 is selected from the following structures: 【Chemistry 6】
7. The method for producing diiodosilane according to claim 1 , wherein the method further comprises reacting hydrogen iodide (HI).
8. 2. The method for producing diiodosilane according to claim 1, wherein the reaction is carried out in a mixed solvent containing an ester-based organic solvent and a halogenated hydrocarbon-based organic solvent.
9. The method for producing diiodosilane according to claim 1, wherein the reaction is carried out at a temperature of 10 to 40°C.
10. 2. The method for producing diiodosilane according to claim 1, further comprising the steps of filtering and purifying the iodate salt by distillation after the reaction.
Citation Information
Patent Citations
Method and equipment for preparing and purifying high-purity diiodosilane
CN117208914A
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JP2019189523A
Producing method of diiodosilane
JP2020063176A
Iodosilane and method for preparing compositions therefrom
JP2023522969A
Method for preparing iodosilane
JP2023548071A