4072-67-7Relevant articles and documents
MICRO-ELECTROLYSIS REACTOR FOR ULTRA FAST, OXIDANT FREE, C-C COUPLING REACTION AND SYNTHESIS OF DACLATASVIR ANALOGS THEREOF
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Paragraph 0152-0157, (2020/12/01)
The present invention relates to a continuous micro-electro-flow reactor system for ultra-fast, oxidant free, C—C coupling reaction for making symmetrical biaryls and analogs thereof. This invention further relates to the said process for preparation of antiviral drug, daclatasvir of general formula I.
Synthesis method of Daclatasvir
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Paragraph 0028; 0041; 0022; 0043; 0051; 0052; 0053, (2016/10/24)
The invention relates to a synthesis method of Daclatasvir. The method comprises the following steps: step 1, performing a bromination reaction on 4.4-diacetyl biphenyl which serves as a raw material so as to obtain an intermediate 1; step 2, performing a substitution reaction on the intermediate 1 so as to obtain an intermediate 2; step 3, performing a cyclization reaction on the intermediate 2 so as to finally obtain the Daclatasvir. Compared with reported synthesis routes, a synthesis route of the method has the following advantages that the route is short, and the yield is high; general means such as suction filtration, extraction and concentration are adopted for aftertreatment, and aftertreatment is simple and convenient; severe-pollution and high-toxicity reagents such as bromine are avoided, and a process of repeatedly using an acetic acid washing reaction system is avoided.
4,4'-bis(2-bromoacetyl) biphenyl synthesizing method
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Paragraph 0028; 0030; 0031, (2017/01/02)
The invention discloses a 4,4'-bis(2-bromoacetyl) biphenyl synthesizing method. The method comprises the following steps of 1, adding methylene dichloride and anhydrous aluminum chloride into a reacting kettle, dropwise adding acetyl chloride after cooling, after finishing adding the acetyl chloride, continuously dropwise adding methylene dichloride solution of biphenyl; 2, warming to carry out friedel-crafts reaction after finishing adding the methylene dichloride solution, adding water after finishing the reaction, concentrating, crystallizing and drying to obtain a product of 4.4-diacetyl biphenyl; 3, adding the 4.4-diacetyl biphenyl into acetic acid and then adding bromine to carry out substitution reaction; 4, filtering, concentrating and crystallizing to obtain the 4,4-bis(2-bromoacetyl) biphenyl after finishing the reaction. By means of the method, the obtained product is higher in both purity and yield.