HRID927140

反应详情

EQUATION

反应方程式

HRID 927140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Prepared as described for 4-hydroxy-6-(2-phenethyl)pyridazin-3(2H)-one (Example 1) from 3,4-bis(benzyloxy)-6-[(3-chloromethyl)phenyl)ethynyl]pyridazine (Intermediate 24) except that the reaction was carried out in ethyl acetate. The crude material was purified by reverse phase chromatography (50 g C18) cartridge eluting with 5-100% acetonitrile/water with acidic modifier and the appropriate fractions combined to give an orange solid. This was recrystallised from ethyl acetate to give a white solid (yield=32%).

WORKUP

后处理

  1. customPrepared
  2. customThe crude material was purified by reverse phase chromatography (50 g C18) cartridge
  3. washeluting with 5-100% acetonitrile/water with acidic modifier
  4. customto give an orange solid
  5. customThis was recrystallised from ethyl acetate