A kind of synthetic method of vemodinil
A technology of vemodinil and a synthesis method, which is applied in the synthesis field of vemodinil, can solve the problems of difficulty in obtaining raw materials, price, harsh reaction conditions, excessively long reaction steps, etc., and achieves a small amount of a reducing agent, a short synthesis route, Environmentally friendly effect
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[0028] The present invention will be described in detail below through examples.
[0029] 1. Synthesis of Intermediate 2
[0030]
[0031] Add 2-chloro-5-nitrophenylboronic acid (0.201g, 1mmol), potassium carbonate (0.138g, 1mmol, 1eq), palladium acetate (0.0112g, 0.05mmol, 5mol%), isopropanol ( In a mixed solvent of 5mL) and water (5mL), after the solid is dissolved, add 2-bromopyridine (0.174g, 1.1mmol, 1.1eq) dropwise under stirring conditions, react at 25℃ for 3h, and extract with ethyl acetate Three times, the obtained organic phases were combined together, added with silica gel and spin-dried, packed in the column by dry method, and passed through the column with petroleum ether: ethyl acetate (v:v=1:1) to obtain the product intermediate 2-(2-chloro-5) -Nitrophenyl)pyridine (2) 0.219g, yield 96%.
[0032] 2. Synthesis of Intermediate 3
[0033]
[0034] Add intermediate 2-(2-chloro-5-nitrophenyl)pyridine (2) (0.114g, 0.5mmol), reducing agent Pd / C (5%Pd) (0.020g), organic base ...
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