HRID1244265

反应详情

EQUATION

反应方程式

HRID 1244265 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 6-chloro-3-[2-(6-fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-4-propyl-pyridazine (268 mg, 0.81 mmol), 3-pyridyl boronic acid (1.84 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), (t-Bu)3P (8 mg, 0.04 mmol) and Cs2CO3 (600 mg, 1.84 mmol) in dioxane (6 mL) is degassed. The mixture is then heated at 100° C. for 6 hours. The solvent is removed in vacuo and water (10 mL) and EtOAc (15 mL) are added. The layers are separated and the aqueous layer is extracted with EtOAc (15 mL). The combined extracts are washed with brine (20 mL), dried (Na2SO4), and evaporated. Preparative TLC purification of the residue provides the title product.

WORKUP

后处理

  1. customis degassed
  2. customThe solvent is removed in vacuo and water (10 mL) and EtOAc (15 mL)
  3. additionare added
  4. customThe layers are separated
  5. extractionthe aqueous layer is extracted with EtOAc (15 mL)
  6. washThe combined extracts are washed with brine (20 mL)
  7. dry with materialdried (Na2SO4)
  8. customevaporated
  9. customPreparative TLC purification of the residue