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Preparation method for 2,2-dimethylol alkanoic acid

A technology of dimethylolalkanoic acid and dimethoxyalkylnitrile, which is applied in the field of preparation of 2,2-dimethylolalkanoic acid, can solve the problem of large amount of waste water, low conversion rate of raw materials, and difficulty in product purification, etc. problem, to achieve the effect of high yield and high purity

Active Publication Date: 2015-04-22
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In summary, the main problems in the existing synthesis process of 2,2-dimethylolalkanoic acid are: low conversion rate of raw materials, difficult to reach 50% product yield, difficult product purification, large amount of waste water generated by operation, Large amount of organic solvents used

Method used

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  • Preparation method for 2,2-dimethylol alkanoic acid
  • Preparation method for 2,2-dimethylol alkanoic acid
  • Preparation method for 2,2-dimethylol alkanoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Dissolve 207g (3.0mol) of n-butyronitrile in 650mL (1040g) of carbon tetrachloride in a 2L three-necked flask equipped with a stirrer, reflux tube, and thermometer, add 246g (6.15mol) of NaOH solid, start stirring and preheat to 50 °C; keep the temperature and add 492 g (6.15 mol) of chloromethyl methyl ether dropwise. After the dropwise addition, the temperature of the reaction system is increased to 80 °C, and the system is kept under reflux for 12 hours.

[0049] After the reaction was finished, excess NaOH and the NaCl produced by the reaction were removed by suction filtration, and the obtained solution was distilled off under reduced pressure to obtain 480 g of concentrated solution. The concentrated solution was dissolved in 250 g of methanol, and 40 wt% of H was added dropwise under agitation. 2 SO 4 Aqueous solution 551.3g (2.25mol), after completion, heated to 70°C for hydrolysis for 5h, after cooling the hydrolyzed solution, 120g of 50wt% NaOH aqueous solutio...

Embodiment 2

[0054] Dissolve 100g (1.8mol) propionitrile in 200mL (180g) tetrahydrofuran (THF) in a 1L three-neck flask equipped with a stirrer, reflux tube, thermometer and inert gas protection, add 423.4g (3.8mol) potassium tert-butoxide at room temperature ), add an ice-water bath, and add 302g (3.8mol) of chloromethyl methyl ether dropwise under full stirring. After the dropwise addition, keep at 0-5°C for 0.5h, remove the ice bath and start heating, and the system is heated to 60°C Reaction 6h.

[0055] After the reaction, the temperature of the system was lowered to room temperature, and H was added dropwise. 2 O6.5g quenches excessive potassium tert-butoxide, stirs 0.2h after adding, adds H 2 0400g dilutes the reaction system, extracts with n-propyl acetate 2 * 350mL, removes the solvent after the organic phase is merged, obtains 280g of viscous concentrated solution, this concentrated solution is dissolved with 140g methanol, drips the H of 40wt% under stirring condition 3 PO 4 ...

Embodiment 3

[0060] Dissolve 100g (1.8mol) of propionitrile in 300mL (280g) of DMF in a 1L three-neck flask equipped with a stirrer, reflux tube, thermometer and inert gas protection, and add 205.2g (3.8mol) of sodium methoxide at room temperature. , add an ice-water bath, add 304g (3.8mol) of chloromethyl methyl ether dropwise under full stirring. After the dropwise addition, keep at 0-5°C for 0.5h, remove the ice bath and start heating to 80°C for 3h.

[0061] After the reaction, the temperature of the system was lowered to room temperature, and H was added dropwise. 2 O6.5g quenches excess sodium methoxide, stirs 0.2h after adding, adds H 2 0600g dilutes the reaction system, extracts with n-propyl acetate 2 * 300mL, removes the solvent after the organic phase is combined, obtains the viscous concentrated solution 265g, and this concentrated solution is dissolved with 120g methanol, drips the HCl aqueous solution 361g of 20wt% under stirring condition, After completion, it was heated to...

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Abstract

The invention relates to a preparation method for 2,2-dimethylol alkanoic acid. The preparation method comprises the following steps: reacting alkylnitrile and chloromethyl methyl ether under the effect of an alkali to generate 2,2-dimethoxy alkylnitrile; carrying out acidic hydrolysis on 2,2-dimethoxy alkylnitrile, so as to obtain the product 2,2-dimethylol alkanoic acid. The process is simple and convenient to react; 2,2-dimethylol alkanoic acid has the advantages of high total yield and high purity; the technical problem that the product is difficult to prepare and purify is overcome.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and more specifically relates to a preparation method of 2,2-dimethylol alkanoic acid. Background technique [0002] Dimethylol alkanoic acid compounds represented by 2,2-dimethylolpropionic acid (DMPA) and 2,2-dimethylolbutyric acid (DMBA) have a special molecular structure: in a quaternary carbon atom There are three different functional groups of hydroxymethyl, carboxyl and alkyl attached to the center. This special molecular structure determines the special chemical properties of such compounds. [0003] Specifically, the multi-substitution structure on the center of the quaternary carbon atom, the covalent bond shape is similar to the tetrahedral configuration in diamond, so that this type of molecule has good photothermal stability; while the lipophilic alkyl group and the hydrophilic hydroxyl group The coexistence of carboxyl and carboxyl groups makes it have unique solubility in oily so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/08C07C59/105C07C59/11
CPCC07C51/08C07C253/30C07C2601/14C07C59/105C07C59/11C07C255/13C07C255/31
Inventor 牟通王漭谢增勇信勇刘运海叶天丛鑫董岩峰朱发明王爱发程英曹善健黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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