HRID1631157
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
- 80 °C
PROCEDURE
实验过程
200 mg of [2-amino-6-(2-chloromethyl-4,5-difluorophenyl)quinazolin-4-yl]-(1,3-dihydroisoindol-2-yl)methanone are dissolved in 5 ml of acetonitrile. 289 mg of caesium carbonate and 84 μl of methylpiperazine are added, and the mixture is stirred at 80° C. for 16 h. After cooling to 25° C., the mixture is filtered, and the filtrate is evaporated to dryness. The residue is taken up in 5 ml of ethyl acetate, the solution is washed with 5 ml of 2N sodium hydroxide solution, and the combined organic phases are dried over sodium sulfate. After filtration, the filtrate is evaporated to dryness and purified by chromatography (reversed phase HPLC).
WORKUP
后处理
- temperatureAfter cooling to 25° C.
- filtrationthe mixture is filtered
- customthe filtrate is evaporated to dryness
- washthe solution is washed with 5 ml of 2N sodium hydroxide solution
- dry with materialthe combined organic phases are dried over sodium sulfate
- filtrationAfter filtration
- customthe filtrate is evaporated to dryness
- custompurified by chromatography (reversed phase HPLC)