HRID729209

反应详情

EQUATION

反应方程式

HRID 729209 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of trans-4-(aminomethyl)cyclohexanecarboxylic acid (10 g, 63.6 mmol, Aldrich) in 2N aqueous NaOH (65 ml) at 0° C. was added benzyl chloroformate (11.9 g, 70 mmol, Aldrich) and the reaction temperature was maintained below 10° C. The cloudy mixture was stirred at RT for 0.5 h. It was then diluted with H2O (100 ml). The clear solution was washed with ether (3×80 ml). The pH of the aqueous layer was adjusted to 2 by adding 6N HCl. The precipitates were filtered and dried in vacuo. 17.8 g of 23 was obtained as a white solid.

WORKUP

后处理

  1. temperaturethe reaction temperature was maintained below 10° C
  2. washThe clear solution was washed with ether (3×80 ml)
  3. additionby adding 6N HCl
  4. filtrationThe precipitates were filtered
  5. customdried in vacuo