HRID31034

反应详情

EQUATION

反应方程式

HRID 31034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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+).

WORKUP

后处理

  1. customAfter evaporation of the volatile components under reduced pressure
  2. customthe phases separated
  3. extractionthe organic layer extracted 5-times with saturated aqueous sodium carbonate
  4. dry with materialAfter drying over magnesium sulphate and evaporation of the solvent