9 results about "Diethyl sulfate" patented technology

The application discloses a preparation method of a key intermediate of dapagliflozin, and belongs to the technical field of preparation of medical intermediates. The preparation method of the key intermediate of dapagliflozin comprises the following steps: 1, 1-ethoxy-4-methylbenzene is prepared by using p-cresol, sodium hydroxide and diethyl sulfate; 2, (4-ethoxybenzyl) phenyl sulfide is prepared by using 1-ethoxy-4-methylbenzene, thiophenol, a palladium catalyst, an alkali and an oxidant; 3, 1-benzyl-4-ethoxybenzene is prepared by using (4-ethoxybenzyl) phenyl sulfide under a hydrogen atmosphere; 4, 4-ethoxy-2'-chlorobenzhydrol is prepared by carrying out chlorination reaction on 1-benzyl-4-ethoxybenzene; and 5, 5-bromo-2-chloro-4'-ethoxybenzhydrol is prepared by carrying out bromination reaction on 4-ethoxy-2'-chlorobenzhydrol. The yield and purity of 5-bromo-2-chloro-4'-ethoxybenzhydrol prepared by the method are higher, the process is safer, and the production cost is reduced.

The invention provides a method for treating excessive halogen in an ionic photoacid generator, which comprises the following steps: adding a crude product of the ionic photoacid generator to be treated into a reactor, adding a solvent, stirring, then adding a sulfate reagent, reacting, then adding an anion raw material, continuing reacting, and after the reaction is completed, carrying out post-treatment to obtain the excessive halogen in the ionic photoacid generator. The ionic photoacid generator with qualified halogen content is obtained. The halogen content is less than or equal to 10 ppm. And the sulfate reagent is dimethyl sulfate, diethyl sulfate, dipropyl sulfate or dibutyl sulfate. The method for treating the residual halogen in the ionic photoacid generator is mild in reaction condition, simple in technological process, environment-friendly and high in yield, and can be widely applied to preparation of iodonium salt and sulfonium salt photoacid generators.

The present invention provides a paroxysmal hemoglobinuria indication drug ipropam key intermediate synthesis method, and relates to the technical field of ipropam, the method comprises: taking p-bromobenzaldehyde as an initial raw material, adopting an organic catalyst to obtain an intermediate 03, carrying out protection group removal on the intermediate 03, carrying out automatic ring closing to obtain an intermediate 04, and carrying out post-treatment to obtain the paroxysmal hemoglobinuria indication drug ipropam key intermediate. Reducing the intermediate 04 with sodium borohydride to obtain a single cis-configuration intermediate 05, then carrying out a chiral flip reaction and hydrolysis to remove p-nitrobenzoic acid, then carrying out an etherification reaction with diethyl sulfate to obtain an intermediate 08, reducing amide of the intermediate 08 with sodium borohydride and boron trifluoride diethyl etherate to obtain an intermediate 09, then carrying out an acetylation reaction to protect amino, and finally carrying out a reaction to obtain the chiral cis-configuration intermediate 03. Cuprous cyanide is subjected to a cyanation reaction and a hydrolytic esterification reaction to obtain the ipropam key intermediate TM. The method is low in raw material price, high in chiral control selectivity, easy in reaction condition control and low in equipment requirement, avoids column chromatography and other operations, and is more suitable for industrial production.

The purpose of the present invention is to provide a treatment agent for production of fibers that achieves both static electricity suppression and flexibility.　Provided is a fiber treatment agent comprising a condensate (A) and a quaternized product (B), wherein: the condensate (A) is at least one compound selected from among condensates (A1) of fatty acid alkanolamide and urea and salts (A2) of the condensates (A1); and the quaternized product (B) is at least one compound selected from among a dimethyl sulfate quaternized product of (poly)oxyalkylene alkyl amine and a diethyl sulfate quaternized product of (poly)oxyalkylene alkyl amine.

The invention discloses a preparation method of a medical intermediate 2-(4-nitrophenyl) butyric acid, and belongs to the technical field of medical fine chemical engineering. According to the method, p-nitrochlorobenzene and alkyl cyanoacetate are used as raw materials to react to prepare an intermediate 2-cyano-2-(4-nitrophenyl) acetoacetate, and then the intermediate 2-cyano-2-(4-nitrophenyl) acetoacetate reacts with diethyl sulfate under the alkaline condition to obtain the 2-cyano-2-(4-nitrophenyl) butyric acid alkyl ester. And finally, hydrolyzing through a concentrated sulfuric acid and acetic acid mixed system to obtain the 2-cyano-2-(4-nitrophenyl) butyric acid. The raw materials and reagents used in the method are cheap and easy to obtain, the process is simple and easy to implement, and the cost advantage is remarkable. Meanwhile, the adopted reaction route does not generate isomeride impurities such as 2-(2-nitrophenyl) butyric acid and the like, the yield is high, and the quality of the obtained product is good.

The invention provides a method for simultaneously preparing nonafluoroisobutyl ether and heptafluoroisobutyrate from bis (heptafluoroisopropyl) heptanone, i.e., the bis (heptafluoroisopropyl) heptanone and fluoroformate react under the catalytic action of alkali metal fluoride to obtain the nonafluoroisobutyl ether and the heptafluoroisobutyrate. The technical scheme provided by the invention has the following advantages: 1) the one-step reaction is realized for the first time to obtain the nonafluoroisobutyl ether and the heptafluoroisobutyrate; the process route is simplified, the equipment investment and the production complexity are reduced, and the technical economy is improved. And 2) compared with the existing nonafluoroisobutyl ether preparation technology, the method does not use a high-toxicity alkylating reagent dimethyl sulfate or diethyl sulfate, does not generate a large amount of difficult-to-treat and high-toxicity solid byproduct potassium methyl sulfate or potassium ethyl sulfate, and is safer and more reliable in process. 3) compared with the existing heptafluoroisobutyrate preparation technology, the technical scheme is simple in process, safe and reliable; the reaction selectivity is good, and byproducts are few; and the product is easy to separate and high in yield.

This invention provides a method for detecting the diethyl sulfate content in methyl 4-acetamido-2-ethoxybenzoate. The method involves derivatizing the sample with sodium iodide-ascorbic acid and detecting the sample using a headspace gas chromatograph equipped with an ECD detector. The chromatographic column is an Agilent DB-624 30m × 0.53mm × 3μm column, the injection port temperature is 220℃, the detector temperature is 250℃, and the carrier gas is N2. 2， Flow rate: 1.5 mL / min, temperature programmed: initial column temperature 70℃, increased to 150℃ at a rate of 5℃ / min and held for 0 min; then run at 240℃ and held for 5 min, flow rate 3 mL / min. This invention provides a convenient, efficient, and accurate method for detecting the diethyl sulfate content in methyl 4-acetamido-2-ethoxybenzoate. This method uses gas chromatography to detect the diethyl sulfate content in methyl 4-acetamido-2-ethoxybenzoate, thereby effectively ensuring medication safety.

The invention discloses a rhodamine esterification method using water as a solvent, and belongs to the technical field of organic synthesis. According to the method, a rhodamine compound as shown in a formula (II) is used as a raw material and reacts with dialkyl sulfate in a water solvent in the presence of an acid-binding agent to generate the rhodamine ester compound as shown in the formula (I). The acid-binding agent is selected from magnesium oxide, calcium oxide and the like, and dialkyl sulfate is dimethyl sulfate or diethyl sulfate; according to the method, water is used for replacing a traditional MIBK solvent, and a byproduct is only alkyl hydrogen sulfate, so that the method is green and environment-friendly; the reaction is free of solvent side reaction interference, the product yield is larger than or equal to 94%, the HPLC purity is larger than or equal to 96%, operation is easy and convenient, cost is low, industrial production is easy, and the method is suitable for the fields of dyes, fluorescent probes and the like.