HRID1079376
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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-(para-fluorophenyl)ethylamine. mp 51°-52° C.
WORKUP
后处理
- customThe reaction was quenched with water
- extractionextracted with 3×100 mL of ethyl acetate
- washThe combined ethyl acetate extracts were washed with 2×100 mL of 5% HCl, water
- dry with materialdried, over Na2SO4
- customEvaporation of the solvent
- customresulted in a yellowish solid which
- customwas purified by recrystallization from ethyl acetate-hexane