HRID915030

反应详情

EQUATION

反应方程式

HRID 915030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
102.5 °C

PROCEDURE

实验过程

A suspension of 5-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-6-phenyl-2,3-pyrazinedicarbonitrile (343 mg) and sodium diformylamide (190 mg) in DMA (1 ml) was heated at 100-105° C. for an hour. After addition of water, the reaction mixture was extracted with CHCl3, dried over MgSO4, concentrated under reduced pressure and subjected to column chromatography on silica gel. With elution of a mixture of n-hexane and EtOAc (50:50 v/v) was obtained [3-cyano-5-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-6-phenyl-2-pyrazinyl]formamide as a solid (30 mg) and with elution of a mixture of n-hexane and EtOAc (30:70 v/v) was obtained [3-cyano-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinyl]-formamide as a solid (22 mg).

WORKUP

后处理

  1. extractionthe reaction mixture was extracted with CHCl3
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated under reduced pressure
  4. washWith elution of a mixture of n-hexane