HRID915040

反应详情

EQUATION

反应方程式

HRID 915040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2-isopropyl-6-{6-[(4-methoxybenzyl)amino]-3-phenyl-2-pyrazinyl}-3(2H)-pyridazinone (2.01 g) in a mixture of toluene (1 ml) and conc. HCl (6 ml) was refluxed for 4 hours. After cooling, an organic layer was removed and an aqueous layer was adjusted to pH 8 with 8N aq. NaOH to yield a precipitate. The precipitate was collected by filtration and dried under reduced pressure and purified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (30:70 v/v) to give 6-(6-amino-3-phenyl-2-pyrazinyl)-2-isopropyl-3(2H)-pyridazinone as a solid (680 mg).

WORKUP

后处理

  1. temperaturewas refluxed for 4 hours
  2. temperatureAfter cooling
  3. customan organic layer was removed
  4. customto yield a precipitate
  5. filtrationThe precipitate was collected by filtration
  6. customdried under reduced pressure
  7. custompurified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (30:70 v/v)