HRID590622

反应详情

EQUATION

反应方程式

HRID 590622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A solution of 2,6-diamino-4-hydroxypyrimidine (CAS: 56-06-4, 1 g, 7.93 mmol) and sodium acetate (0.85 g, 10.32 mmol) in water (180 mL) was stirred at 100° C. for 30 minutes. Methyl 4-(2-bromoacetyl)benzoate (2.24 g, 8.72 mmol) was suspended in MeOH (25 mL) and was added slowly to the above solution. The reaction mixture was then stirred at 100° C. for 16-20 h and then cooled to room temperature. The residue was filtered and dried. It was then stirred in CH2Cl2 (10 mL) and filtered to provide XI-8-I (1.07 g, 47.5%). LCMS: m/z 285 (M+1)+.

WORKUP

后处理

  1. additionwas added slowly to the above solution
  2. temperaturecooled to room temperature
  3. filtrationThe residue was filtered
  4. customdried
  5. stirringIt was then stirred in CH2Cl2 (10 mL)
  6. filtrationfiltered
  7. customto provide XI-8-I (1.07 g, 47.5%)