HRID234836

反应详情

EQUATION

反应方程式

HRID 234836 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionis added upon which all solid
  2. customThe dichloromethane layer is separated
  3. extractionthe aqueous phase extracted with dichloromethane (3×8 mL)
  4. dry with materialThe extracts are dried over magnesium sulfate
  5. customremoved under a slow nitrogen stream