反应详情

温度

80 °C

To 300 mg (0.77 mmol) of (8-bromo-1-methyl-1,2,3,4-tetrahydrobenzo[e][1,4]diazepin-5-ylidenemethyl)phosphonic acid diethyl ester (prepared as described in Example 41) in 1 ml of dioxane was added 123 mg (0.81 mmol) of 3-methoxyphenylboronic acid, 7.8 mg (0.028 mmol) of tricyclohexylphosphine, 10.5 mg 0.012 mmol) of tris-(dibenzylideneacetone)-palladium (0) and 141 mg of caesium fluoride. The mixture was heated at 80° C. for 6 hours. The mixture was partitioned between ethyl acetate and water. The organic phase was evaporated and the product was purified by column chromatography (20 g IST pre-packed column) eluting with acetone—petroleum ether (40-60° C.) (1:2) to give 217 mg of [8-(3-methoxyphenyl)-1-methyl-1,2,3,4-tetrahydrobenzo[e][1,4]diazepin-5-ylidenemethyl]phosphonic acid diethyl ester as a yellow gum; MS: m/e 417 (M+).

1. customThe mixture was partitioned between ethyl acetate and water
2. customThe organic phase was evaporated
3. customthe product was purified by column chromatography (20 g IST pre-packed column)
4. washeluting with acetone—petroleum ether (40-60° C.) (1:2)