反应详情

A solution of 1,1-dimethylethyl 4-{4-[3-(methyloxy)-4-nitrophenyl]-3-cyclohexen-1-yl}-1-piperazinecarboxylate (0.75 g, 1.80 mmol, combined batches) was stirred at rt under N2 in 20% TFA in DCM (40 mL) for approximately 2 h. The solution was then concentrated under vacuum. The residue was dissolved in DCM and aqueous (saturated) NaHCO3. The aqueous layer was separated and extracted with DCM (3×). The combined organic layers were dried over MgSO4, filtered, then concentrated and purified by silica gel chromatography to give the title compound of step F (446 mg, 1.40 mmol, 78%) as a light tan solid. MS (ESI): 318 [M+H]+.

1. concentrationThe solution was then concentrated under vacuum
2. dissolutionThe residue was dissolved in DCM
3. customThe aqueous layer was separated
4. extractionextracted with DCM (3×)
5. dry with materialThe combined organic layers were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified by silica gel chromatography