HRID1061875

反应详情

EQUATION

反应方程式

HRID 1061875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 1-methyl-6-[(1-trityl-1H-imidazol-4-yl)carbonyl]-2-naphthyl trifluoromethanesulfonate (26.8 g), triethylamine (15.7 mL), methanol (50 mL), palladium acetate (0.61 g), 1,1′-bis(diphenylphosphino)ferrocene (1.50 g) and DMF (150 mL) was stirred under a carbon monooxide atmosphere with heating at 70° C. for 16 hrs. The reaction mixture was cooled and diluted with water (1.6 L). The precipitate was collected by filtration and purified by column chromatography (carrier: silica gel, developing solvent: ethyl acetate). The obtained crystal was washed with diisopropyl ether and dried to give the title compound (20.9 g) as-colorless crystals.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. filtrationThe precipitate was collected by filtration
  3. custompurified by column chromatography (carrier: silica gel, developing solvent: ethyl acetate)
  4. washThe obtained crystal was washed with diisopropyl ether
  5. customdried