HRID409495

反应详情

EQUATION

反应方程式

HRID 409495 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 trans-4-[(tert-Butoxycarbonyl)(methyl)amino]cyclohexanecarboxylic acid methyl ester (3.69 mmol, 1.0 g) is dissolved in EtOAc (5 mL), cooled to 0° C. and treated with 4M HCl in ethyl acetate (5 mL). The mixture is stirred at room temperature for 5 hours. After the mixture is concentrated under reduced pressure, 100 mL of ethyl ether is added. The solid precipitate is filtrated, washed with ethyl ether and dried under reduced pressure to obtain 700 mg (91%) of trans-4-(methylamino)cyclohexanecarboxylic acid methyl ester hydrochloride as white solid. ESI-MS m/z: 171 [M+1]+, Retention time 1.00 min (condition B).

WORKUP

后处理

  1. concentrationAfter the mixture is concentrated under reduced pressure, 100 mL of ethyl ether
  2. additionis added
  3. filtrationThe solid precipitate is filtrated
  4. washwashed with ethyl ether
  5. customdried under reduced pressure