반응 #600987

반응 방정식

2-amino-N-(7-chloro-4-methoxy-quinolin-8-yl)-benzenesulfonamide

ammonium formate

→

title compound

수율 32.2%

2-Amino-N-(4-methoxy-quinolin-8-yl)-benzenesulfonamide

수율 32.2%

용매

AcOH

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   기타the solvent was removed in vacuo
3. 3
   workup.DISSOLUTIONThe residue was dissolved in EtOAc (100 ml)
4. 4
   세척the organic phase was washed with sat. NaHCO3 solution (50 ml)
5. 5
   건조dried (MgSO4)
6. 6
   농축concentrated in vacuo
7. 7
   기타The crude residue was purified by column chromatography DCM/MeOH (99:1) as the eluent

실험 절차

10% Pd—C (97 mg) was added to a solution of 2-amino-N-(7-chloro-4-methoxy-quinolin-8-yl)-benzenesulfonamide 570 (470 mg, 1.8 mmol), ammonium formate (571 mg, 9.2 mmol) in 50% AcOH (10 ml) and the mixture was heated to 70° C. for 15 h. After cooling, the solvent was removed in vacuo. The residue was dissolved in EtOAc (100 ml) and the organic phase was washed with sat. NaHCO3 solution (50 ml), dried (MgSO4) concentrated in vacuo. The crude residue was purified by column chromatography DCM/MeOH (99:1) as the eluent to give the title compound (191 mg, 32%).

출처