HRID2420206

反应详情

EQUATION

反应方程式

HRID 2420206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 68.4 g. of 2-amino-5-methyl-4,6-dichloro-phenol hydrochloride and 96 ml. of N,N-diethylaniline in 750 ml. of acetone, 23.4 ml. of acetyl chloride were added slowly by keeping the temperature under 20° C. At the end, the reaction mixture was heated to reflux for an hour. After cooling, the solution was poured into water; the solid product, thus obtained, was collected on a buckner, washed with water until the washings were neutral and dried in a desicator at 50° C. The raw product obtained was purified by crystallization from ethyl alcohol, yielding 44 g. of a pure product with M.P. = 175°-176.5° C.

WORKUP

后处理

  1. additionTo a mixture of 68.4 g
  2. customunder 20° C
  3. temperatureAt the end, the reaction mixture was heated
  4. temperatureto reflux for an hour
  5. temperatureAfter cooling
  6. customthe solid product, thus obtained
  7. customwas collected on a buckner
  8. washwashed with water until the washings
  9. customdried in a desicator at 50° C