反应详情

温度

20 °C

To a solution of cis-N-Isopropyl-4-(5-(methylsulfonyl)-2-nitrophenylamino)cyclohexanecarboxamide (0.120 g, 0.313 mmol) in MeOH (1.2 mL) was added 5% Pd/C (0.067 g, 0.031 mmol) and ammonium formate (0.154 mL, 3.13 mmol) (exotherm). The reaction mixture was stirred at 20° C. for 1 hour and then the mixture was filtered through a pad of Celite® brand filter aid, washing with MeOH. The filtrate was concentrated under vacuum, and the remaining residue was dissolved in DCM then washed with water. The organic layer was concentrated under vacuum. The residue was purified by flash chromatography, eluting with 0-80% 90:10:1 DCM/MeOH/NH4OH:DCM to afford cis-4-(2-amino-5-(methylsulfonyl) phenylamino)-N-isopropylcyclohexanecarboxamide as a pale yellow oil (0.107 g, 97% yield). MS (ESI pos. ion) m/z: 354.2 [M+H].

1. filtrationthe mixture was filtered through a pad of Celite® brand
2. filtrationfilter aid
3. washwashing with MeOH
4. concentrationThe filtrate was concentrated under vacuum
5. dissolutionthe remaining residue was dissolved in DCM
6. washthen washed with water
7. concentrationThe organic layer was concentrated under vacuum
8. customThe residue was purified by flash chromatography
9. washeluting with 0-80% 90:10:1 DCM/MeOH/NH4OH