HRID931301

反应详情

EQUATION

反应方程式

HRID 931301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrogen chloride gas was bubbled into a solution of 4-methylpiperidine-3-carboxylic acid (6.0 g, 41.90 mmol) in ethanol (150 mL) and acetic acid (30 mL) at 0° C. under a nitrogen atmosphere. The reaction mixture was heated at reflux for 48 h, then was cooled and was partitioned between water and ethyl acetate. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to afford ethyl 4-methylpiperidine-3-carboxylate (5.0 g). The material was used without further purification.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 48 h
  3. temperaturewas cooled
  4. customwas partitioned between water and ethyl acetate
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure