Water → N-[5-[4-(5-{[(2R,6S)-2,6-Dimethyl-4-morpholinyl]methyl}-1,3,4-oxadiazol-2-yl)-1-(phenylsulfonyl)-1H-indazol-6-yl]-2-(methyloxy)-3-pyridinyl]-2,4-difluorobenzenesulfonamide

HRID 38835

反応式

HRID 38835 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[S:9](Cl)(=[O:11])=[O:10].[CH3:13][C@H:14]1[O:19][C@@H:18]([CH3:20])[CH2:17][N:16]([CH2:21][C:22]2[O:26][C:25]([C:27]3[CH:35]=[C:34]([C:36]4[CH:37]=[C:38]([NH2:44])[C:39]([O:42][CH3:43])=[N:40][CH:41]=4)[CH:33]=[C:32]4[C:28]=3[CH:29]=[N:30][N:31]4[S:45]([C:48]3[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=3)(=[O:47])=[O:46])=[N:24][N:23]=2)[CH2:15]1.O>N1C=CC=CC=1>[CH3:13][C@H:14]1[O:19][C@@H:18]([CH3:20])[CH2:17][N:16]([CH2:21][C:22]2[O:26][C:25]([C:27]3[CH:35]=[C:34]([C:36]4[CH:37]=[C:38]([NH:44][S:9]([C:3]5[CH:4]=[CH:5][C:6]([F:8])=[CH:7][C:2]=5[F:1])(=[O:11])=[O:10])[C:39]([O:42][CH3:43])=[N:40][CH:41]=4)[CH:33]=[C:32]4[C:28]=3[CH:29]=[N:30][N:31]4[S:45]([C:48]3[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=3)(=[O:46])=[O:47])=[N:24][N:23]=2)[CH2:15]1

参加物

5

反応物 3

HCID 962WaterHCID 27342732,4-Difluorobenzenesulfonyl Chloride2 回HCID 666916425-[4-(5-{[(2R,6S)-2,6-Dimethyl-4-morpholinyl]methyl}-1,3,4-oxadiazol-2-yl)-1-(phenylsulfonyl)-1H-indazol-6-yl]-2-(methyloxy)-3-pyridinamine

生成物 1

HCID 66691781N-[5-[4-(5-{[(2R,6S)-2,6-Dimethyl-4-morpholinyl]methyl}-1,3,4-oxadiazol-2-yl)-1-(phenylsulfonyl)-1H-indazol-6-yl]-2-(methyloxy)-3-pyridinyl]-2,4-difluorobenzenesulfonamide収率 80.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

2,4-Difluorobenzenesulfonyl chloride (0.048 mL, 0.354 mmol) was added dropwise to a solution of 5-[4-(5-{[(2R,6S)-2,6-dimethyl-4-morpholinyl]methyl}-1,3,4-oxadiazol-2-yl)-1-(phenylsulfonyl)-1H-indazol-6-yl]-2-(methyloxy)-3-pyridinamine (185 mg, 0.321 mmol) in pyridine (1 ml). The mixture was stirred at room temperature for 2 h. 2,4-Difluorobenzenesulfonyl chloride (0.048 mL, 0.354 mmol) was added dropwise and the mixture continued stirring at room temperature for 1 h. Water (10 ml) was added and the resultant brown precipitate collected by filtration and dried in the vacuum oven for 72 h to give the title compound as a brown solid (194 mg).

後処理

  1. stirringthe mixture continued stirring at room temperature for 1 h
  2. filtrationthe resultant brown precipitate collected by filtration
  3. customdried in the vacuum oven for 72 h

出典と根拠

ORDレコード
ord-f59b3f5990294c9d9cc102117b1d7a29
出典データセット
uspto-grants-2013_09
特許番号
US08524751B2

関連ノート

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