HRID515250

反应详情

EQUATION

反应方程式

HRID 515250 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

60% sodium hydride (12.0 g, 0.30 mol) was suspended in THF (300 mL) and cooled down to 0° C. 4-amino-6-bromo-2-methylpyrimidine (Compound 9) (18.7 g, 0.1 mol) was then added in batches and stirred for 30 min. After methyl 2-chlorothiazole-5-formate (Compound 10) (17.7 g, 0.1 mol) was added in batches, the reactants were heated and reacted by refluxing for 4 h, and then cooled down to room temperature for reaction overnight. When controlling the temperature between 0° C. and 5° C., hydrochloric acid (2N) was added for neutralization reaction. After adding keep heat and stirred to grow grains for 1 h. Filtrate and wash the cake with water, and then dry to give target Compound 11 (25.8 g, yield is 78.4%).

WORKUP

后处理

  1. temperaturethe reactants were heated
  2. customreacted
  3. temperatureby refluxing for 4 h
  4. temperaturecooled down to room temperature for reaction overnight
  5. additionwas added for neutralization reaction
  6. additionAfter adding keep
  7. temperatureheat
  8. stirringstirred
  9. customfor 1 h
  10. washFiltrate and wash the cake with water
  11. customdry