Water → N-[2,4-difluoro-3-(5-pyridin-3-yl 1-triisopropylsilanyl-1H-pyrrolo[2,3-b]pyridine-3-carbonyl)-phenyl]-ethanesulfonamide

HRID 1098374ノート

反応式

HRID 1098374 の反応式
[NH2:1][C:2]1[C:3]([F:36])=[C:4]([C:9]([C:11]2[C:19]3[C:14](=[N:15][CH:16]=[C:17]([C:20]4[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=4)[CH:18]=3)[N:13]([Si:26]([CH:33]([CH3:35])[CH3:34])([CH:30]([CH3:32])[CH3:31])[CH:27]([CH3:29])[CH3:28])[CH:12]=2)=[O:10])[C:5]([F:8])=[CH:6][CH:7]=1.[CH3:37][S:38](Cl)(=[O:40])=[O:39].[CH2:42](N(CC)CC)C.O>C(Cl)Cl>[F:36][C:3]1[C:4]([C:9]([C:11]2[C:19]3[C:14](=[N:15][CH:16]=[C:17]([C:20]4[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=4)[CH:18]=3)[N:13]([Si:26]([CH:30]([CH3:32])[CH3:31])([CH:33]([CH3:35])[CH3:34])[CH:27]([CH3:28])[CH3:29])[CH:12]=2)=[O:10])=[C:5]([F:8])[CH:6]=[CH:7][C:2]=1[NH:1][S:38]([CH2:37][CH3:42])(=[O:40])=[O:39]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 59506753(3-amino-2,6-difluoro-phenyl)-(5-pyridin-3-yl-1-triisopropylsilanyl-1H-pyrrolo[2,3-b]pyridin-3-yl)-methanone

生成物 1

HCID 59506897N-[2,4-difluoro-3-(5-pyridin-3-yl 1-triisopropylsilanyl-1H-pyrrolo[2,3-b]pyridine-3-carbonyl)-phenyl]-ethanesulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To (3-amino-2,6-difluoro-phenyl)-(5-pyridin-3-yl-1-triisopropylsilanyl-1H-pyrrolo[2,3-b]pyridin-3-yl)-methanone (57, 35.0 mg, 0.069 mmol) in methylene chloride (6 mL) was added methanesulfonyl chloride (0.30 mL, 3.9 mmol) and triethylamine (0.40 mL, 2.9 mmol). The reaction was stirred at room temperature overnight. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated to give the crude compound that was used in the next step.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-827b71ab34914e51bfd5ebabc8b70daf
出典データセット
uspto-grants-2012_03
特許番号
US08143271B2

反応ノート

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