172529-93-0Relevant articles and documents
Preparation method of 3-(butoxy (methyl) phosphoryl)-1-cyanopropyl acetate
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Paragraph 0025-0043, (2021/10/02)
The invention relates to a preparation method of 3-(butoxy (methyl) phosphoryl)-1-cyano propyl acetate. According to the invention, a mixture in a reactor is evaporated to a water segregator and a mixture in a water segregator flows back to the reactor at the same time, so that the consumption of a catalyst and the methyl monobutyl hypophosphite is greatly reduced. Meanwhile, the unit operation of high-vacuum evaporation of the methyl monobutyl hypophosphite is omitted, the production process is simplified, and the production cost is reduced; furthermore, when the mass content of the product in the reactor is greater than or equal to 96.5%, the product in the reactor is extracted while evaporation reflux is kept between the reactor and the water segregator, so that the reaction can be continuously carried out, and continuous production of the product is realized; the preparation method disclosed by the invention is simple to operate, green and environment-friendly, low in cost and high in yield.
Preparation method of penciclovir
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, (2020/02/14)
The invention discloses a preparation method of penciclovir. An existing synthetic route mainly has the following defects that the N-7 site by-products need to be removed through column chromatography, a large amount of three wastes are generated, and the yield of N-9 site products is not high. According to the technical scheme adopted by the invention, the preparation method comprises the following steps: carrying out alkylation on 2-amino-6-chloropurine and triethyl bromopropane under an alkaline condition to introduce an N-9 site side chain, carrying out decarboxylation and transesterification in a methanol solution of sodium methoxide to generate the 2-amino-6-chloro-9-(3,3-dimethoxycarbonyl-1-propyl)purine; then reducing the 2-amino-6-chloro-9-(3,3-dimethoxycarbonyl-1-propyl)purine togenerate 2-amino-6-chloro-9-(3-hydroxymethyl-4-hydroxy-1-butyl)purine with sodium borohydride; and finally, directly hydrolyzing under acidic conditions to obtain penciclovir. According to the method, the target product is obtained by directly hydrolyzing the reduction product, ester group protection and deprotection are not needed, and the method has the advantages of few reaction steps, good product quality, simplicity and convenience in operation, suitability for industrial production and the like.
Method for synthesizing glufosinate ammonium salt
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Paragraph 0103; 0108-0110; 0123; 0128-0130; 0137; 0142-0144, (2019/11/13)
The invention discloses a method for synthesizing a glufosinate ammonium salt. The method comprises the following steps that (1) methyldiethoxyphosphine and n-butanol are used as raw materials to produce an intermediate I by hydrolysis and transesterification; (2) the intermediate I is subjected to a free radical addition reaction with acrolein cyanohydrin acetate to form an intermediate II; (3) the intermediate II is subjected to an aminolysis reaction with ammonia gas to form a mixture of an intermediate III and an intermediate IV; (4) the intermediate III and the intermediate IV are subjected to acid hydrolysis with hydrochloric acid to form an intermediate V; and (5) the intermediate V is neutralized, purified and crystallized to obtain the glufosinate ammonium salt. The method does not need to use toxic raw materials, avoids the large-scale use of ammonia water and ammonium chloride, not only greatly reduces the safety hazard, but also reduces the quantity of by-products and the amount of waste water generated, and the environmental protection risk is greatly reduced; and the purification process is simple, the product content and the yield coefficient are obviously increased,and the method is suitable for industrial scale production.