Dimethylamine → HCID 11612472, 화합물

HRID 2267511노트

반응식

HRID 2267511 반응식
NS(N)(=O)=O.Cl[CH2:7][CH2:8][CH2:9][S:10]([N:13]1[CH2:18][CH2:17][CH:16]([C:19]2[C:27]3[C:22](=[C:23]([C:34]([NH2:36])=[O:35])[CH:24]=[C:25]([C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[CH:26]=3)[NH:21][CH:20]=2)[CH2:15][CH2:14]1)(=[O:12])=[O:11].[CH3:37][NH:38][CH3:39].C([O-])([O-])=O.[K+].[K+].[Na+].[I-]>>[CH3:37][N:38]([CH3:39])[CH2:7][CH2:8][CH2:9][S:10]([N:13]1[CH2:18][CH2:17][CH:16]([C:19]2[C:27]3[C:22](=[C:23]([C:34]([NH2:36])=[O:35])[CH:24]=[C:25]([C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[CH:26]=3)[NH:21][CH:20]=2)[CH2:15][CH2:14]1)(=[O:12])=[O:11]

참가 물질

6

반응물 5

HCID 674DimethylamineHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 82267SulfamideHCID 590032803-{1-[(3-chloropropyl)sulfonyl]-4-piperidinyl}-5-phenyl-1H-indole-7-carboxamide

생성물 1

HCID 11612472HCID 11612472, 화합물수율 19%

실험 절차

Following the general procedure for aminosulfonamide formation outlined in example 2, 3-{1-[(3-chloropropyl)sulfonyl]-4-piperidinyl}-5-phenyl-1H-indole-7-carboxamide (47 mg, 0.1 mmol) and dimethylamine (2.0M in THF, 0.5 mL, 0.5 mmol), were allowed to react in the presence of K2CO3 (55.2 mg, 0.4 mmol) and NaI (Cat. 1.51 mg). The resulting residue was purified by reverse phase HPLC eluting with 10% B to 80% B, where A=H2O (0.1% trifluoroacetic acid) and B=CH3CN (0.1% trifluoroacetic acid) to give the title compound (8.7 mg, 19%).

후처리

  1. customThe resulting residue was purified by reverse phase HPLC
  2. washeluting with 10% B to 80% B, where A=H2O (0.1% trifluoroacetic acid) and B=CH3CN (0.1% trifluoroacetic acid)

출처 및 근거

ORD 기록
ord-fcda699514f1431c8f5d6ef702bc867c
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858796B2

반응 노트

불러오는 중…