HRID1815825

反应详情

EQUATION

反应方程式

HRID 1815825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 20.0 gm (70.4 mMol) 1-benzyl-3-methoxycarbonyl-4-oxopiperidine hydrochloride in 60 mL ethylene glycol was cooled in an ice bath as 24 gm hydrogen chloride were added. The slurry was heated at 70° C. for 2 hours and was then poured into 200 mL ice water. The pH was adjusted to about 8 with 5N sodium hydroxide and the resulting mixture extracted well with diethyl ether. The organic extracts were combined, dried over sodium sulfate, and concentrated under reduced pressure to provide 21 gm 8-benzyl-8-azaspiro[4,5]decane-6-carboxylic acid methyl ester.

WORKUP

后处理

  1. additionwere added
  2. extractionthe resulting mixture extracted well with diethyl ether
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure