HRID127357

反应详情

EQUATION

反应方程式

HRID 127357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 600 ml of acetone, 31.5 g of 2-chloro-3-pyridinecarboxylic acid is added and suspended by stirring. Triethylamine (40 ml) is added and after 30 minutes 42.6 g of 3-bromophthalide is poured with stirring into the resulting reaction mixture. The mixture is refluxed for 4 hours and then poured into 2000 ml of water at 50° C. To obtain a precipitated compound, the reaction mixture is cooled with continuous stirring. The solid precipitate is collected by filtration, washed with cooled water and then dried under vacuum at a temperature of 40° C. A yield of 38.7 g (67% of theory) of phthalidyl 2-chloro-3-pyridinecarboxylate is obtained (m.p. 137°-8° C.).

WORKUP

后处理

  1. additionis poured
  2. stirringwith stirring into the resulting reaction mixture
  3. temperatureThe mixture is refluxed for 4 hours
  4. customTo obtain a precipitated compound
  5. temperaturethe reaction mixture is cooled with continuous stirring
  6. filtrationThe solid precipitate is collected by filtration
  7. washwashed with cooled water
  8. customdried under vacuum at a temperature of 40° C