反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe reactants were heated
- customreacted
- temperatureby refluxing for 4 h
- temperaturecooled down to room temperature for reaction overnight
- additionwas added for neutralization reaction
- additionAfter adding keep
- temperatureheat
- stirringstirred
- customfor 1 h
- washFiltrate and wash the cake with water
- customdry