HRID349116
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
[2-(3-Benzyloxy-5-fluoro-phenyl)-1-oxiranyl-ethyl]-carbamic acid tert-butyl ester (3.33 g, 8.59 mmol) and m-ethyl benzylamine (2.32 g, 17.19 mmol) were dissolved in isopropyl alcohol (80 ml) and brought to reflux for 2 h. Reaction mixture was then concentrated in vacuo to remove isopropyl alcohol. Dissolved yellow liquid in ethyl acetate (30 ml), then washed with 1N HCl (3×100 ml). Aqueous layers were combined then extracted with ethyl acetate (2×100 ml). Organic layers were washed with 10% sodium bicarbonate (aq., 3×100 ml), followed by a brine wash. Organic layer was dried over sodium sulfate, filtered, then concentrated in vacuo, yielding the product (4.31 g). (ES+: 523.9)
WORKUP
后处理
- temperatureto reflux for 2 h
- customReaction mixture
- concentrationwas then concentrated in vacuo
- customto remove isopropyl alcohol
- dissolutionDissolved yellow liquid in ethyl acetate (30 ml)
- washwashed with 1N HCl (3×100 ml)
- extractionAqueous layers were combined then extracted with ethyl acetate (2×100 ml)
- washOrganic layers were washed with 10% sodium bicarbonate (aq., 3×100 ml)
- washwash
- dry with materialOrganic layer was dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo