HRID234831

反应详情

EQUATION

反应方程式

HRID 234831 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe dark solution obtained
  2. concentrationit is concentrated to dryness
  3. custompartitioned between brine (30 mL) and ethyl acetate (2×25 mL)
  4. customThe orange-red solid insoluble in the biphasic mixture is separated by suction filtration
  5. customdried at 40° C. under vacuum (0.43 g)