HRID2354420

反应详情

EQUATION

反应方程式

HRID 2354420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe reaction flask was capped by a rubber septum
  2. temperaturethe reaction mixture was maintained at room temperature for 48 h
  3. concentrationThe reaction mixture was concentrated
  4. customthe residue was partitioned between EtOAc
  5. washThe organic layer was washed by brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated