반응 #59312

반응 방정식

Carbonic acid (S)-1-[(S)-5-(2-benzyloxy-ethyl)-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-ylcarbamoyl]-ethyl ester 4-nitro-phenyl ester

2-fluoroethylamine hydrochloride

→

title compound

(2-Fluoro-ethyl)-carbamic acid (S)-1-[(S)-5-(2-benzyloxy-ethyl)-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-ylcarbamoyl]-ethyl ester

용매

pyridine

반응 조건

후처리

1. 1
   기타After evaporation of the volatile components under reduced pressure
2. 2
   기타the phases separated
3. 3
   추출the organic layer extracted 5-times with saturated aqueous sodium carbonate
4. 4
   건조After drying over magnesium sulphate and evaporation of the solvent

실험 절차

Carbonic acid (S)-1-[(S)-5-(2-benzyloxy-ethyl)-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-ylcarbamoyl]-ethyl ester 4-nitro-phenyl ester (80 mg, 0.13 mmol), 2-fluoroethylamine hydrochloride (40 mg, 0.40 mmol) and pyridine (2 ml) were stirred in a sealed tube for 18 h at ambient temperature. After evaporation of the volatile components under reduced pressure, the residue was taken up in water/ethyl acetate, the phases separated and the organic layer extracted 5-times with saturated aqueous sodium carbonate, twice with 10% citric acid and once with saturated aqueous sodium chloride. After drying over magnesium sulphate and evaporation of the solvent, the title compound is obtained as white solid (>98%). MS: n/e=520(M+H+).

출처