HRID2164299

反应详情

EQUATION

反应方程式

HRID 2164299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 60 g (0.2 mole) of 7-(2-fluorobenzoyl)-3-methylthioindolin-2-one and 60 g (0.5 mole) of tin powder in one liter of 95% ethanol was heated to reflux and 150 ml of concentrated hydrochloric acid was added. Heating was continued for 18 hrs, then the mixture was cooled and the precipitate was collected by decanting the slurry from the remaining tin and filtering the slurry. The filter cake was recrystallized twice from absolute ethanol to give 31 g (60%) white needles, m.p. 209°-210° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux
  3. temperatureHeating
  4. temperaturethe mixture was cooled
  5. customthe precipitate was collected
  6. customby decanting the slurry from the remaining tin
  7. filtrationfiltering the slurry
  8. customThe filter cake was recrystallized twice from absolute ethanol