反応 #657330

反応方程式

benzyl chloroformate

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

sodium bicarbonate

→

tan solid

収率 104.5%

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

収率 104.5%

溶媒

THF

反応条件

後処理

1. 1
   その他then partitioned between ethyl acetate (200 mL) and water (100 mL)
2. 2
   その他The organic layer was separated
3. 3
   洗浄washed with saturated brine solution (200 mL)
4. 4
   乾燥dried (MgSO4)
5. 5
   ろ過filtered
6. 6
   濃縮concentrated

実験手順

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.

出典