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
- 95 °C
PROCEDURE
实验过程
To a solution of methyl 3-(3,4,5,6-tetramethoxy-2-methylbenzyl)-2-(trifluoromethanesulfonyl)oxybenzoate (316 mg, 0.6220 mmol) in toluene (7.1 ml) were added tetrakistriphenylphosphine palladium (22 mg, 0.0190 mmol), aqueous solution of sodium carbonate (2M aqueous solution, 0.81 ml), lithium chloride (53 mg, 1.2502 mmol) and ethanolic solution (1.3 ml) of pyridine-3-boronic acid 1,3-propanediol cyclic ester (151 mg, 0.9320 mmol) and the mixture was heated with stirring at 95° C. for 16 hours. The reaction solution was diluted with ethyl acetate (100 ml), washed with water and dried and the solvent was evaporated therefrom. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to give the title compound (231 mg, 0.5286 mmol, 85%).
WORKUP
后处理
- temperaturethe mixture was heated
- washwashed with water
- customdried
- customthe solvent was evaporated
- customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)