HRID359408

反应详情

EQUATION

反应方程式

HRID 359408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 152 parts of 3-methyl-1-(phenylmethyl)-4-piperidinone in 900 parts of methylbenzene were added dropwise 218 parts of ethyl carbonochloridate at room temperature. Upon completion, stirring was continued overnight at reflux. After cooling the reaction mixture was washed with water and hydrochloric acid, dried, filtered and evaporated. The residue was distilled, yielding 120.5 parts (83%) of ethyl 3-methyl-4-oxo-1-piperidinecarboxylate; bp. 98°-105° C. at 1 mm pressure (intermediate 26).

WORKUP

后处理

  1. temperatureat reflux
  2. temperatureAfter cooling the reaction mixture
  3. washwas washed with water and hydrochloric acid
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. distillationThe residue was distilled