HRID1061875
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was cooled
- filtrationThe precipitate was collected by filtration
- custompurified by column chromatography (carrier: silica gel, developing solvent: ethyl acetate)
- washThe obtained crystal was washed with diisopropyl ether
- customdried