HRID632132

反应详情

EQUATION

反应方程式

HRID 632132 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

6-Bromo-5-cyclopentyl-pyridine-2-carboxylic acid methyl ester (0.6 g, 2.1 mmol), bis(diphenylphosphino)ferrocene-palladium(II)dichloride methylene chloride complex (CAN 95464-05-4, 90 mg, 0.11 mmol) and potassium carbonate (0.37 g, 2.68 mmol) were added to a solution of 3-chlorophenylboronic acid (CAN 63503-60-6, 0.42 g, 2.69 mmol) in water (20 mL) and DMF (2 mL). The mixture was stirred for 48 h at 100° C. Its pH was adjusted to pH=3 with diluted hydrochloric acid. The mixture was extracted with methylene chloride (3×20 mL). The organic layers were combined, dried over sodium sulfate and concentrated under reduced pressure to give the title compound (130 mg, 20%) which was used in the next step without further purification; MS (EI): m/e=302.0 [M+H]+.

WORKUP

后处理

  1. extractionThe mixture was extracted with methylene chloride (3×20 mL)
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under reduced pressure