反应 #657330

反应方程式

benzyl chloroformate

4-amino-piperidine-1-carboxylic acid tert-butyl ester

sodium bicarbonate

→

tan solid

收率 104.5%

4-Benzyloxycarbonylamino-piperidine-1-carboxylic acid tert-butyl ester

收率 104.5%

溶剂

THF

反应条件

后处理

1. 1
   其他then partitioned between ethyl acetate (200 mL) and water (100 mL)
2. 2
   其他The organic layer was separated
3. 3
   洗涤washed with saturated brine solution (200 mL)
4. 4
   干燥dried (MgSO4)
5. 5
   过滤filtered
6. 6
   浓缩concentrated

实验过程

To a solution of 4-amino-piperidine-1-carboxylic acid tert-butyl ester (11.98 g, 58.4 mmol, 1 equiv) in THF (80 mL) at 23° C. was added a saturated solution of sodium bicarbonate (200 mL) followed by benzyl chloroformate (9.19 mL, 64.2 mmol, 1.1 equiv). The reaction was stirred for 55 min then partitioned between ethyl acetate (200 mL) and water (100 mL). The organic layer was separated, washed with saturated brine solution (200 mL), dried (MgSO4), filtered and concentrated to give 20.4 g of tan solid. This material was used in the next step without further purification.

来源