HRID1614212
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
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
- customIn a 500-cm3 ground-necked flask surmounted by a condenser
- customplaced in an oil bath
- customis stabilized at 60° C
- additionAfter the addition
- waitthe mixture is then left
- stirringstirring vigorously for 30 hours
- additionby pouring it into ice-cold water
- customthe precipitate obtained
- washwashed with water until the filtrate
- customThe product is dried
- customrecrystallized in absolute ethanol