HRID2120555

反应详情

EQUATION

反应方程式

HRID 2120555 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

To a solution of n-butanol (0.633 g, 8.54 mmol) in anhydrous DMF (50 mL) at 0° C. under the N2, NaH (0.307 g, 12.8 mmol) was added quickly. The obtained suspension was stirred for 0.5 h at 0° C. 2,4-Dichloro-6-(morpholin-4-yl)pyrimidine (2 g, 8.54 mmol) was added to the suspension. After the suspension was warmed to room temperature and stirred for 12 h, the reaction mixture was quenched with ice/brine and extracted with 200 mL EtOAc. The extract was washed with brine, and dried over Na2SO4. The solvent was removed under reduced pressure. The crude residue was purified using flash chromatography (silica; EtOAc/Hexane: 1/6) to yield 1.4 g of 2-n-butoxy-4-chloro-6-(morpholin-4-yl)pyrimidine (white solid, 60%).

WORKUP

后处理

  1. temperatureAfter the suspension was warmed to room temperature
  2. stirringstirred for 12 h
  3. customthe reaction mixture was quenched with ice/brine
  4. extractionextracted with 200 mL EtOAc
  5. washThe extract was washed with brine
  6. dry with materialdried over Na2SO4
  7. customThe solvent was removed under reduced pressure
  8. customThe crude residue was purified