HRID729072

反应详情

EQUATION

反应方程式

HRID 729072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. waitat 20° C. for eighteen hours
  2. customis flushed out into an absorption trap with a stream of nitrogen
  3. customThe solid precipitate is removed by filtration
  4. washwashed twice with methyl ethyl ketone
  5. customdried with suction
  6. customto yield 13.7 grams (52% yield) of the titlecompound which melts at 113-114° C.