反应详情

温度

80 °C

A mixture of 1-(4-bromobenzyl)-6-phenylmethoxy-2-(4-fluorophenyl)-1,2,3,4-tetrahydroisoquinoline (1.0 g, 1.99 mmol), dibenzylideneacetone palladium (36 mg, 0.04 mmol), BINAP (74 mg, 0.12 mmol), sodium tert-butoxide (0.29 g, 3.0 mmol) and N-acetylpiperazine (0.38 g, 3.0 mmol) in 2 ml of toluene were added to a sealed tube under an argon atmosphere and heated at 80° C. for 16 h. The sealed tube was cooled to room temperature and the contents of the tube transferred to a separatory funnel. Ethyl acetate and water were added and the organic layer was separated. The combined organic layers were dried over MgSO4, concentrated, and purified by column chromatography (SiO2, chloroform/methanol, 99:1) to provide the title compound (0.45 g, 41% yield): ES-MS (m/z) 550 [M+H]+.

1. additionwere added to a sealed tube under an argon atmosphere
2. temperatureThe sealed tube was cooled to room temperature
3. customthe contents of the tube transferred to a separatory funnel
4. customthe organic layer was separated
5. dry with materialThe combined organic layers were dried over MgSO4
6. concentrationconcentrated
7. custompurified by column chromatography (SiO2, chloroform/methanol, 99:1)