HRID594091

反应详情

EQUATION

反应方程式

HRID 594091 的结构方程式

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 2,6-dichloro-4-methoxypyridine (1.0 equiv.) and morpholine (20 equiv.) were heated to 130° C. for 40 min in the microwave. The reaction mixture was centrifuged and the soluble portion was removed from solids. Water was added to the soluble portion which resulted in precipitation of product. This mixture was centrifuged and the soluble portion was discarded. The remaining solids were partitioned between water and EtOAc. The organic phase was washed with brine and dried over sodium sulfate. The solution was concentrated and dried under vacuo to give 4-(6-chloro-4-methoxypyridin-2-yl)morpholine in 43% yield. LCMS (m/z) (M+H)=229.1, Rt=0.76 min.

WORKUP

后处理

  1. customthe soluble portion was removed from solids
  2. additionWater was added to the soluble portion which
  3. customresulted in precipitation of product
  4. customThe remaining solids were partitioned between water and EtOAc
  5. washThe organic phase was washed with brine
  6. dry with materialdried over sodium sulfate
  7. concentrationThe solution was concentrated
  8. customdried under vacuo