反应详情

A solution of [2-(4-chloro-phenyl)-2,4,5,6,7,8-hexahydro-cycloheptapyrazol-3-yl]-cyclohexyl-acetic acid ethyl ester (337 mg, 812 umol) in MeOH (19 ml) and 4 N aqueous NaOH (3.05 ml, 12.2 umol) was heated for 14 h under reflux conditions. The solvent was removed under reduced pressure, ice water/2 N aqueous HCl solution/iPrOAc 1/1/2 was added and the layers were separated. The aqueous layer was extracted one more time with iPrOAc. The combined extracts were washed with ice water/brine 1/1 and dried over Na2SO4. After filtration the solvent was removed under reduced pressure to give the title compound (284 mg, 734 umol; 90%) as off-white solid which was sufficiently pure to be used in the next step. MS: m/e=387.2 [M+H

1. customThe solvent was removed under reduced pressure, ice water/2 N aqueous HCl solution/iPrOAc 1/1/2
2. additionwas added
3. customthe layers were separated
4. extractionThe aqueous layer was extracted one more time with iPrOAc
5. washThe combined extracts were washed with ice water/brine 1/1
6. dry with materialdried over Na2SO4
7. filtrationAfter filtration the solvent
8. customwas removed under reduced pressure