反应 #1435768

反应方程式

(S)-3-(2-Amino-4-fluoro-phenoxy)-2-tert-butoxycarbonylamino-propionic acid

N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimid-hydrochloride

→

((S)-2-fluoro-8-oxo-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocyclohepten-7-yl)-carbamic acid tert-butyl ester

收率 86.0%

溶剂

dimethylformamide

反应条件

后处理

1. 1
   萃取Extraction
2. 2
   其他with water/ethylacetate and removal of the solvent
3. 3
   workup.DISTILLATIONby distillation

实验过程

1.96 g (6.24 mmol) (S)-3-(2-Amino-4-fluoro-phenoxy)-2-tert-butoxycarbonylamino-propionic acid and 1.20 g (6.24 mmol) N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimid-hydrochloride in 25 ml dimethylformamide were stirred overnight at room temperature. Extraction with water/ethylacetate and removal of the solvent by distillation yielded 1.58 g (86%) ((S)-2-fluoro-8-oxo-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocyclohepten-7-yl)-carbamic acid tert-butyl ester, MS m/e (%): 314 (M+NH4+, 13), 297 (M+H+, 40), 241 (100), 197 (63).

来源