HRID234831
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
A suspension of 2-[2-(N-tert-butoxycarbonylamino)ethyl]-5-(p-toluenesulfonyl oxy)isoquino[8,7,6cd]indazole-6(2H)-one Example 3 (0.535 g) and N-(tert-butoxycarbonyl)ethylenediamine (1.12 g) in dry pyridine (5.35 mL) is heated at 80° C. The dark solution obtained is held at this temperature for 5 hours, then it is concentrated to dryness and partitioned between brine (30 mL) and ethyl acetate (2×25 mL). The orange-red solid insoluble in the biphasic mixture is separated by suction filtration and dried at 40° C. under vacuum (0.43 g).
WORKUP
后处理
- customThe dark solution obtained
- concentrationit is concentrated to dryness
- custompartitioned between brine (30 mL) and ethyl acetate (2×25 mL)
- customThe orange-red solid insoluble in the biphasic mixture is separated by suction filtration
- customdried at 40° C. under vacuum (0.43 g)