HRID408808

反应详情

EQUATION

反应方程式

HRID 408808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Heat a solution of 4,6-dichloro-2-methyl-pyrimidin-5-ylamine (5.0 g, 0.02 mol), 2-methoxyethylamine (2.32 g, 0.03 mol) and diisopropylethylamine (3.9 g, 0.03 mol) in isopropanol (70 mL) at 150° C. in a sealed tube for 16 h. Cool the reaction mixture to room temperature, and remove the isopropanol under reduced pressure to give a residue. Dissolve the residue in dichloromethane and wash with water and brine. Dry the organic layer over anhydrous sodium sulfate, filter, and concentrate under reduced pressure to give a residue. Purify the residue on a silica gel column eluting with methanol:dichloromethane (4:96) to give the title compound (5.0 g). ES/MS m/z 217 (M+1).

WORKUP

后处理

  1. customremove the isopropanol under reduced pressure
  2. customto give a residue
  3. washwash with water and brine
  4. dry with materialDry the organic layer over anhydrous sodium sulfate
  5. filtrationfilter
  6. concentrationconcentrate under reduced pressure
  7. customto give a residue
  8. customPurify the residue on a silica gel column
  9. washeluting with methanol:dichloromethane (4:96)