反应详情

Benzylchloroformate (8.6 ml, 60 mmol) was added to a stirred mixture of 3-bromopropylamine hydrobromide (6.6 g, 30 mmol) in methylene chloride (100 ml) and 3N sodium hydroxide solution (100 ml) at 0° C. After stirring two phase reaction mixture at room temperature for overnight, organic layer was separated and washed with water twice (30 ml×2). After drying with MgSO4, the volatile solvent was evaporated under reduced pressure. The residue was purified with silica gel column chromatography (EtOAc:Hx=1:4) to obtain desire compound (8.6 g, 98%) as colorless oil.

1. customtwo phase reaction mixture at room temperature for overnight
2. customorganic layer was separated
3. washwashed with water twice (30 ml×2)
4. dry with materialAfter drying with MgSO4
5. customthe volatile solvent was evaporated under reduced pressure
6. customThe residue was purified with silica gel column chromatography (EtOAc:Hx=1:4)