HRID869134

反应详情

EQUATION

反应方程式

HRID 869134 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (2-(4-fluorophenyl)-2-methylpropan-1-amine (27 g, 160 mmol, 1.6 equiv), 3,6-dichloropyridazine (15 g, 100 mmol, 1.0 equiv) and K2CO3 (42 g, 302 mmol, 3.0 equiv) in isopropanol (15 mL) was stirred at 100° C. for 36 hours. The cooled mixture was partitioned between water and EtOAc and the organic fraction was dried over Na2SO4 and concentrated in vacuo. Partial purification over silica gel using a 30-75% gradient of EtOAc/hexanes gave the desired product (29.6 g, 103%) which was used without further purification.

WORKUP

后处理

  1. customThe cooled mixture was partitioned between water and EtOAc
  2. dry with materialthe organic fraction was dried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customPartial purification over silica gel using a 30-75% gradient of EtOAc/hexanes