Triethylamine → 3,3a,4,5-Tetrahydro-3a-methoxycarbonyl-N-[4-(trifluoromethyl)phenyl]-N-(dibutylaminosulfenyl)-2H-benz[g]indazole-2-carboxamide

HRID 232727

반응식

HRID 232727 반응식
[CH3:1][O:2][C:3]([C:5]12[CH2:13][CH2:12][C:11]3[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=3[C:9]1=[N:8][N:7]([C:18]([NH:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=1)=[O:19])[CH2:6]2)=[O:4].C(N(CC)CC)C.[CH2:38]([N:42]([CH2:45][CH2:46][CH2:47][CH3:48])[S:43]Cl)[CH2:39][CH2:40][CH3:41]>C(Cl)Cl>[CH3:1][O:2][C:3]([C:5]12[CH2:13][CH2:12][C:11]3[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=3[C:9]1=[N:8][N:7]([C:18]([N:20]([C:21]1[CH:22]=[CH:23][C:24]([C:27]([F:30])([F:28])[F:29])=[CH:25][CH:26]=1)[S:43][N:42]([CH2:45][CH2:46][CH2:47][CH3:48])[CH2:38][CH2:39][CH2:40][CH3:41])=[O:19])[CH2:6]2)=[O:4]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 81031Amidosulfenyl chloride, N,N-dibutyl-HCID 189883493,3a,4,5-tetrahydro-3a-methoxycarbonyl-N-[4'-(trifluoromethyl)phenyl]-2H-benz[g]indazole-2-carboxamide

생성물 1

HCID 233594573,3a,4,5-Tetrahydro-3a-methoxycarbonyl-N-[4-(trifluoromethyl)phenyl]-N-(dibutylaminosulfenyl)-2H-benz[g]indazole-2-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of the title compound of Step B (Example 1) (0.4 g, 0.96 mmol) in 8 ml methylene chloride cooled to 0° C. was added triethylamine (0.15 g) and dibutylaminosulfenylchloride (0.2 g). The reaction mixture was, warmed to room temperature and stirred for one hour. The mixture was subjected to silica gel column chromatography using hexane-ether (6:1) as the eluent. The title compound was obtained (0.24 g) in high purity.

출처 및 근거

ORD 기록
ord-a077c5948d0f48569018d4e31e151f72
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591764

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