HRID558227

反应详情

EQUATION

反应方程式

HRID 558227 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the stirred solution of 6-azido-4-(4-bromo-2-fluoro-phenylamino)-6-chloro-pyridazine-3-carboxylic acid tert-butyl ester (122 mg, 0.30 mmol) in 5 ml of mixed solvents (3:1 v/v, dichloromethane/acetic acid) is added zinc powder (98 mg, 1.5 mmol) at room temperature. After three hours, the reaction mixture is poured into ethyl acetate (50 ml). The organic layer is washed with water, saturated NaHCO3 (30 ml×3) and saturated NaCl (30 ml×3). The organic layer is dried over Na2SO4, and concentrated. The residue is purified by flash column chromatography to provide the desired product.

WORKUP

后处理

  1. washThe organic layer is washed with water, saturated NaHCO3 (30 ml×3) and saturated NaCl (30 ml×3)
  2. dry with materialThe organic layer is dried over Na2SO4
  3. concentrationconcentrated
  4. customThe residue is purified by flash column chromatography