HRID127357
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
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
- additionis poured
- stirringwith stirring into the resulting reaction mixture
- temperatureThe mixture is refluxed for 4 hours
- customTo obtain a precipitated compound
- temperaturethe reaction mixture is cooled with continuous stirring
- filtrationThe solid precipitate is collected by filtration
- washwashed with cooled water
- customdried under vacuum at a temperature of 40° C