HRID1096994

反应详情

EQUATION

反应方程式

HRID 1096994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewith heating
  2. temperatureunder reflux
  3. customEthanol was removed from the reaction solution under reduced pressure
  4. additionthe residue was diluted with water
  5. additionadded
  6. filtrationthe formed precipitate was taken out through filtration
  7. washwashed with methanol and ethyl acetate in that order
  8. customdried under reduced pressure