HRID2047498

反应详情

EQUATION

反应方程式

HRID 2047498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A suspension of 2,6-difluoro-N-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-benzamide (359 mg, 1 mmol), 3-bromo-4-methyl-benzoic acid methyl ester (228 mg, 1 mmol), benzyl(chloro)bis(triphenylphosphine)palladium (38 mg, 0.05 mmol) and K2CO3 (690 mg, 5 mmol) in 1-methylpyrrolidinone (NMP) (5 ml) was degassed with vacuum and heated at 120° C. for 10 hr. After cooling down to room temperature, ethyl acetate (EtOAc) (200 ml) was added and the mixture was washed with water (60 ml×3). The EtOAc was evaporated and the residue was purified by column chromatography on silica gel (Hexanes:EtOAc) to give Compound 1 (286 mg, yield 75%).

WORKUP

后处理

  1. customwas degassed with vacuum
  2. temperatureAfter cooling down to room temperature
  3. additionethyl acetate (EtOAc) (200 ml) was added
  4. washthe mixture was washed with water (60 ml×3)
  5. customThe EtOAc was evaporated
  6. customthe residue was purified by column chromatography on silica gel (Hexanes:EtOAc)