HRID1636432

反应详情

EQUATION

反应方程式

HRID 1636432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Butanethiol (0.39 ml) was added dropwise to a solution of sodium (0.08 g) in ethanol (3 ml). The solution was stirred for 1/2 hour and then added slowly to a refluxing solution of 6-bromo-4-chloro-3-propyl-2H-1-benzopyran-2-one (1 g) in ethanol (4 ml). The mixture was heated under reflux for 41/2 hours, filtered hot through kieselguhr and the filtrate allowed to cool. The precipitate was purified by silica gel column chromatography to give 6-bromo-4-butylthio-3-propyl-2H-1-benzopyran-2-one, m.p. 62-4° (compound 15)

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 41/2 hours
  3. filtrationfiltered hot through kieselguhr
  4. temperatureto cool
  5. customThe precipitate was purified by silica gel column chromatography