HRID326237

反应详情

EQUATION

反应方程式

HRID 326237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 500-cm3 ground-necked flask surmounted by a condenser, and placed in an oil bath, 40.8 g (0. 15 mol) of 6-(bromoacetyl)benzothiazolinone are dissolved in 90 cm3 of trifluoroacetic acid with magnetic stirring and while the temperature is stabilized at 60° C. 52.7 cm3 (0-33 mol) of triethylsilane are introduced dropwise via a dropping funnel. After the addition, the heating is stopped and the mixture is then left stirring vigorously for 30 hours. The reaction medium is hydrolyzed by pouring it into ice-cold water, and the precipitate obtained is drained and washed with water until the filtrate is neutral and then with hexane. The product is dried and recrystallized in absolute ethanol.

WORKUP

后处理

  1. customIn a 500-cm3 ground-necked flask surmounted by a condenser
  2. customplaced in an oil bath
  3. customis stabilized at 60° C
  4. additionAfter the addition
  5. waitthe mixture is then left
  6. stirringstirring vigorously for 30 hours
  7. additionby pouring it into ice-cold water
  8. customthe precipitate obtained
  9. washwashed with water until the filtrate
  10. customThe product is dried
  11. customrecrystallized in absolute ethanol