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
PROCEDURE
实验过程
To a mixture of 10-(p-methoxybenzyloxy)-5-[[2-(dimethylamino)ethyl]amino]-2-methylisoquino[5,6,7-cd]indazole-6(2H)-one of Example 28(0.010 g) in dichloromethane (1 mL) trifluoroacetic acid is added upon which all solid is in solution. After 1 h the mixture is diluted with dichloromethane (3 mL) and a saturated solution of sodium bicarbonate (5 mL) is added. The dichloromethane layer is separated and the aqueous phase extracted with dichloromethane (3×8 mL). The extracts are dried over magnesium sulfate and removed under a slow nitrogen stream. The material is placed under vacuum for 2 h to give 5-[[2-(dimethylamino)ethyl]amino]-2-methyl-10-hydroxyisoquino[5,6,7-cd]indazole-6(2H)-one as an amorphous solid.
WORKUP
后处理
- additionis added upon which all solid
- customThe dichloromethane layer is separated
- extractionthe aqueous phase extracted with dichloromethane (3×8 mL)
- dry with materialThe extracts are dried over magnesium sulfate
- customremoved under a slow nitrogen stream