HRID1162988
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
- 160 °C
PROCEDURE
实验过程
(2-Chloro-9-cyclopentyl-purin-6-yl)-{2-[3-(4-methyl-piperazin-1-yl)-propoxy]-phenyl}-amine (0.1 mmol), sodium cyanide (50 mg), potassium iodide (5 mg) are suspended in DMA (2 ml) and heated up to 160° C. and the mixture is stirred at this temperature for 24 hours. The mixture is diluted with water and extracted 3 times with ethyl acetate. The combined organic phases are washed with brine and the extract is dried over sodium sulfate and evaporated. The residue is dissolved in diethylether, filtered over powdered charcoal and cooled to 4° C. The solid material formed is filtered of and dried (vacuum). A white powder with mp. 136-138° C. is obtained.
WORKUP
后处理
- extractionextracted 3 times with ethyl acetate
- washThe combined organic phases are washed with brine
- dry with materialthe extract is dried over sodium sulfate
- customevaporated
- dissolutionThe residue is dissolved in diethylether
- filtrationfiltered over powdered charcoal
- temperaturecooled to 4° C
- customThe solid material formed
- filtrationis filtered of and
- customdried (vacuum)
- customA white powder with mp. 136-138° C. is obtained