反応式
[CH2:1]([C:5]1[N:6]([CH2:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[S:34](=[O:37])(=[O:36])[NH2:35])=[CH:24][CH:23]=2)[C:7](=[O:20])[N:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:16]([F:19])([F:18])[F:17])[N:9]=1)[CH2:2][CH2:3][CH3:4].[CH3:38][S:39]([C:42]1[CH:50]=[CH:49][C:45]([C:46](O)=[O:47])=[CH:44][CH:43]=1)(=[O:41])=[O:40]>>[CH2:1]([C:5]1[N:6]([CH2:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[S:34](=[O:37])(=[O:36])[NH:35][C:46](=[O:47])[C:45]3[CH:44]=[CH:43][C:42]([S:39]([CH3:38])(=[O:41])=[O:40])=[CH:50][CH:49]=3)=[CH:24][CH:23]=2)[C:7](=[O:20])[N:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:16]([F:19])([F:18])[F:17])[N:9]=1)[CH2:2][CH2:3][CH3:4]参加物
3
反応物 2
生成物 1
実験手順
The title compound was prepared from 5-n-butyl-2,4-dihydro-4-[(2'-sulfamoylbiphenyl-4-yl)methyl]-2-[2-(trifluoromethyl)phenyl]-3H-1,2,4-triazol-3-one (from Example 16, Step C), according to the procedure of Example 43 except that p-(methylsulfonyl)benzoic acid was used as the acid. The crude product was purified by flash chromatography (gradient elution using 0.5-10% MeOH/CH2Cl2) to afford a 60% yield of the desired compound as a white solid, homogeneous by TLC in 5% MeOH/CH2Cl2 ; mass spectrum (FAB) m/e 735 (M+Na)+, 751 (M+K)+ ; mp 131°-133° C.
後処理
- customThe crude product was purified by flash chromatography (gradient elution using 0.5-10% MeOH/CH2Cl2)
出典と根拠
- ORDレコード
- ord-bb129c8ee71f47c58862a26c4ee156ff
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05411980
関連ノート
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