反应详情

(4-Chloro-phenyl)-hydrazine (100 mg, 700 μmol; CAS Reg. No. 1073-69-4) was added to a solution of 2-cyclohexyl-3-oxo-3-(2-oxo-cyclohexyl)-propionic acid ethyl ester (206 mg, 700 μmol) in ethanol (4.7 ml). The reaction mixture was heated under reflux conditions for 6 h. The solvent was removed under reduced pressure. The residue was taken up in ice water/brine 1/1 and extracted two times 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 a brown oil which was purified by preparative thick layer chromatography (silica gel, iPrOAc/heptane) to give the title compound (130 mg, 324 μmol; 46%) as orange solid. MS: m/e=401.2 [M+H+].

1. temperatureThe reaction mixture was heated under reflux conditions for 6 h
2. customThe solvent was removed under reduced pressure
3. extractionextracted two times with iPrOAc
4. washThe combined extracts were washed with ice water/brine 1/1
5. dry with materialdried over Na2SO4
6. filtrationAfter filtration the solvent
7. customwas removed under reduced pressure
8. customto give a brown oil which
9. customwas purified by preparative thick layer chromatography (silica gel, iPrOAc/heptane)