反应详情

温度

80 °C

To a solution of cyclohexyl-(2-phenyl-2H-indazol-3-yl)-amine (30 mg, 103 μmol) in chloroform was added Et3N (16 μl, 113 μmol) and cyclohexylacetylchloride (16 μl, 108 μmol; CAS Reg. No. 23860-35-7) at ambient temperature under an argon atmosphere. The mixture was heated to 80° C. for 12 h, poured onto ice water/1 N HCl 1/1 and extracted two times with iPrOAc. The combined extracts were washed with ice water/1 N NaOH 1/1 and ice water/brine 1/1 and dried over Na2SO4. After filtration the solvent was removed under reduced pressure and the crude product was purified by preparative thin layer chromatography (silica gel, iPrOAc/heptane) to give the title compound (27 mg, 65 μmol; 63%) as colorless foam. MS: m/e=416.5 [M+H+].

1. customat ambient temperature
2. extractionextracted two times with iPrOAc
3. washThe combined extracts were washed with ice water/1 N NaOH 1/1 and ice water/brine 1/1
4. dry with materialdried over Na2SO4
5. filtrationAfter filtration the solvent
6. customwas removed under reduced pressure
7. customthe crude product was purified by preparative thin layer chromatography (silica gel, iPrOAc/heptane)