反应 #816391
ord-4d3827e9f07a4901b599d9d062a73bc6
反应方程式
trans-4-(aminomethyl)cyclohexanecarboxylic acid
benzyl chloroformate
→
23
收率 96.1%
4-{[(phenylmethoxy)carbonylamino]methyl}cyclohexanecarboxylic acid
收率 96.1%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度the reaction temperature was maintained below 10° C
- 2洗涤The clear solution was washed with ether (3×80 ml)
- 3workup.ADDITIONby adding 6N HCl
- 4过滤The precipitates were filtered
- 5其他dried in vacuo
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.