HRID931137

反应详情

EQUATION

反应方程式

HRID 931137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-bromo-5-cyanopyridine (1 g, 5.3 mmol) in tetrahydrofuran was added cyclopropyl boronic acid (0.5 g, 5.6 mmol) and potassium phosphate (1.08 g, 15.9 mmol). The resulting solution was degassed with nitrogen for 10 minutes and then palladium (II) acetate and S-phos were added. The reaction mixture was refluxed for 16 h. The reaction mixture was diluted with water, extracted with ethyl acetate and concentrated under reduced pressure. The crude material was purified via column chromatography to afford 5-cyclopropylnicotinonitrile (0.45 g, 58%). MS (ES+) (M+H) 145.1774.

WORKUP

后处理

  1. customThe resulting solution was degassed with nitrogen for 10 minutes
  2. additionpalladium (II) acetate and S-phos were added
  3. temperatureThe reaction mixture was refluxed for 16 h
  4. additionThe reaction mixture was diluted with water
  5. extractionextracted with ethyl acetate
  6. concentrationconcentrated under reduced pressure
  7. customThe crude material was purified via column chromatography