反应详情

温度

95 °C

A solution of methyl vinyl sulfone (201 mg, 1.89 mmol) and 1-{4-[3-(methyloxy)-4-nitrophenyl]-3-cyclohexen-1-yl}piperazine (200 mg, 0.63 mmol) was stirred in dioxane (6 mL) under N2. The reaction was then heated to 95° C. and stirred for approximately 3 h. The reaction was then cooled to rt and concentrated under vacuum. The residue was taken up in DCM and aqueous (saturated) NaHCO3. The aqueous layer was extracted with DCM (2×). The combined organic layers were dried over MgSO4, filtered, then concentrated and purified by silica gel chromatography to give the title compound of step G (222 mg, 0.52 mmol, 83%) as a light yellow solid. MS (ESI): 424 [M+H]+.

1. temperatureThe reaction was then cooled to rt
2. concentrationconcentrated under vacuum
3. extractionThe aqueous layer was extracted with DCM (2×)
4. dry with materialThe combined organic layers were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified by silica gel chromatography