HRID2354420
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Crude 4-[(2R)-2-(4-Bromophenyl)-2-chloroethyl]morpholine (34.5 g) was dissolved in 200 mL of EtOH at room temperature with magnetic stirring. The resulting solution was cooled to 0° C. and treated with 71 ml of MeNH2 (33 wt % in EtOH) under N2. The reaction flask was capped by a rubber septum, and the reaction mixture was maintained at room temperature for 48 h. The reaction mixture was concentrated, and the residue was partitioned between EtOAc and sat NaHCO3(aq). The organic layer was washed by brine, dried over MgSO4, and filtered. The filtrate was concentrated to yield the title compound as a yellow solid (31.6 g, 93%). MS (ES) m/e 300, 301 [M+H]+.
WORKUP
后处理
- customThe reaction flask was capped by a rubber septum
- temperaturethe reaction mixture was maintained at room temperature for 48 h
- concentrationThe reaction mixture was concentrated
- customthe residue was partitioned between EtOAc
- washThe organic layer was washed by brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationThe filtrate was concentrated