HRID1096994
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a 1.0-liter egg plant-type flask, mercaptoacetic acid (10.3 g, 0.15 mol) and potassium hydroxide (35.6 g, 0.54 mol) were added to an ethanol (600 mL) solution of 5-chloro-3-methyl-1-pyridin-2-yl-1H-pyrazole-4-carbaldehyde (30.0 g, 0.14 mol), and stirred for 2 hours with heating under reflux. Ethanol was removed from the reaction solution under reduced pressure, then the residue was diluted with water and made acidic with aqueous 5 N hydrochloric acid solution added thereto, and the formed precipitate was taken out through filtration, washed with methanol and ethyl acetate in that order, and dried under reduced pressure to obtain the title compound as a pale brown solid.
WORKUP
后处理
- temperaturewith heating
- temperatureunder reflux
- customEthanol was removed from the reaction solution under reduced pressure
- additionthe residue was diluted with water
- additionadded
- filtrationthe formed precipitate was taken out through filtration
- washwashed with methanol and ethyl acetate in that order
- customdried under reduced pressure