HRID916662

反应详情

EQUATION

反应方程式

HRID 916662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of 3-bromo-2-(1H-imidazol-2-yl)-pyridine (prepared from 3-bromo-pyridine-2-carbonitrile essentially as described by Clews et al., Synthesis (2001):1549) (675 mg, 3 mmol), zinc cyanide (223 mg, 1.9 mmol), Pd2(dba)3 (137 mg, 0.15 mmol), DPPF (160 mg, 0.3 mmol) and water (0.2 mL) in DMF (15 mL) is degassed with argon for 15 minutes. The mixture is then heated at 40° C. overnight in a sealed tube. Solvent is removed, water (30 mL) is added and the mixture is extracted with methylene chloride. On drying (MgSO4), the solvent is removed and the resulting solid is washed with ether (5×10 mL) to give the product (170).

WORKUP

后处理

  1. customas described by Clews et al., Synthesis (2001)
  2. customSolvent is removed
  3. additionwater (30 mL) is added
  4. extractionthe mixture is extracted with methylene chloride
  5. dry with materialOn drying (MgSO4)
  6. customthe solvent is removed
  7. washthe resulting solid is washed with ether (5×10 mL)