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
- 90 °C
PROCEDURE
实验过程
Next, 3-chloro-4-{4-[5-(3-{[glycyl(methyl)amino]methyl}phenyl)pyrimidin-2-yl]piperazin-1-yl}benzoic acid (2 g) was suspended in THF (40 ml)-H2O (40 ml), and fumaric acid (938 mg) was added thereto, followed by stirring at 90° C. for 1 hour. The reaction mixture was cooled to room temperature and the solvent was evaporated under reduced pressure. To the residue was added THF (20 ml)-H2O (20 ml), followed by stirring at 90° C. for 1 hour as it was suspended. The mixture was cooled to room temperature, followed by stirring overnight. After the mixture was filtered, washed with THF—H2O (1:1), and then dried at 50° C. for 5 hours under reduced pressure to obtain 3-chloro-4-{4-[5-(3-{[glycyl(methyl)amino]methyl}phenyl)pyrimidin-2-yl]piperazin-1-yl}benzoic acid hemifumarate (1.7 g) as a colorless crystal.
WORKUP
后处理
- additionwas added
- temperatureThe reaction mixture was cooled to room temperature
- customthe solvent was evaporated under reduced pressure
- additionTo the residue was added THF (20 ml)-H2O (20 ml)
- stirringby stirring at 90° C. for 1 hour as it
- temperatureThe mixture was cooled to room temperature
- stirringby stirring overnight
- filtrationAfter the mixture was filtered
- washwashed with THF—H2O (1:1)
- customdried at 50° C. for 5 hours under reduced pressure