HRID1653687

反应详情

EQUATION

反应方程式

HRID 1653687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzylchloroformate (12.2 g, 72 mmol) was added dropwise to a stirred solution, at 0° C., of 4-fluorophenylethyl amine (9.42 g, 72 mmol) in 50 mL of DMF. The mixture was stirred for an additional 3 hours at the same temperature. The reaction was quenched with water and extracted with 3×100 mL of ethyl acetate. The combined ethyl acetate extracts were washed with 2×100 mL of 5% HCl, water and dried over Na2SO4. Evaporation of the solvent resulted in a yellowish solid which was purified by recrystallization from ethyl acetate-hexane to furnish 8.6 g (46% yield) of N-Benzyloxycarbonyl-2-(parafluorophenyl)ethylamine. mp 51°-52° C.

WORKUP

后处理

  1. customThe reaction was quenched with water
  2. extractionextracted with 3×100 mL of ethyl acetate
  3. washThe combined ethyl acetate extracts were washed with 2×100 mL of 5% HCl, water
  4. dry with materialdried over Na2SO4
  5. customEvaporation of the solvent
  6. customresulted in a yellowish solid which
  7. customwas purified by recrystallization from ethyl acetate-hexane