HRID729072
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A solution of 19.9 grams (0.1 mol) of 1-acetyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 150 ml of dry methyl ethyl ketone is added dropwise at 0° C over a 30-minute period to asolution of 28 ml (approximately 0.4 mol) of phosgene in 150 ml of methyl ethyl ketone. The reaction mixture is stirred at 0° C for one hour,then at 20° C. for eighteen hours. Excess dissolved phosgene is flushed out into an absorption trap with a stream of nitrogen. The solid precipitate is removed by filtration, washed twice with methyl ethyl ketone and dried with suction to yield 13.7 grams (52% yield) of the titlecompound which melts at 113-114° C.
WORKUP
后处理
- waitat 20° C. for eighteen hours
- customis flushed out into an absorption trap with a stream of nitrogen
- customThe solid precipitate is removed by filtration
- washwashed twice with methyl ethyl ketone
- customdried with suction
- customto yield 13.7 grams (52% yield) of the titlecompound which melts at 113-114° C.