HRID42231

反应详情

EQUATION

反应方程式

HRID 42231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

7-Chloro-4-[4-(5-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-1H-imidazo[4,5-d]pyridazine (149 mg, 0.389 mmol), benzyl zinc bromide (9.34 mL, 0.5M in THF, 4.67 mmol), and tetrakis (triphenylphosphine) palladium0 (23 mg, 0.020). The reaction mixture is heated to 80° C. for 32 h. Add H2O and extract product with EtOAc. Wash combined organics with brine and concentrate in vacuo. The residue is purified by flash chromatography on silica gel (60-100% EtOAc/Heptane flushed with 10% MeOH/EtOAc) to afford the title compound (12.1 mg, 7%).

WORKUP

后处理

  1. extractionAdd H2O and extract product with EtOAc
  2. washWash
  3. concentrationconcentrate in vacuo
  4. customThe residue is purified by flash chromatography on silica gel (60-100% EtOAc/Heptane flushed with 10% MeOH/EtOAc)