反応式
CCCC[N+](CCCC)(CCCC)CCCC.[F-].[F:19][C:20]([Si](C)(C)C)([F:22])[F:21].[Cl:27][C:28]1[C:33]([CH:34]=[O:35])=[CH:32][C:31]([C:36]#[N:37])=[CH:30][C:29]=1[NH:38][C:39]1[N:44]=[C:43]([NH:45][CH:46]2[CH2:48][CH2:47]2)[C:42]2=[N:49][CH:50]=[C:51]([C:52]#[N:53])[N:41]2[N:40]=1>C1COCC1>[Cl:27][C:28]1[C:33]([CH:34]([OH:35])[C:20]([F:22])([F:21])[F:19])=[CH:32][C:31]([C:36]#[N:37])=[CH:30][C:29]=1[NH:38][C:39]1[N:44]=[C:43]([NH:45][CH:46]2[CH2:48][CH2:47]2)[C:42]2=[N:49][CH:50]=[C:51]([C:52]#[N:53])[N:41]2[N:40]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
TBAF (1 M in THF, 0.026 mL, 0.026 mmol) was added to a suspension of (trifluoromethyl)trimethylsilane (2 M solution in THF, 0.079 mL, 0.16 mmol) and 2-((2-chloro-5-cyano-3-formylphenyl)amino)-4-(cyclopropylamino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (20 mg, 0.053 mmol) in dry THF (1 mL) under nitrogen in an ice bath. The bath was removed and the reaction was left stirring at room temperature overnight. Aqueous 1 N HCl was added and the reaction was left stirring for 20 min. This was neutralized with 1.3 N potassium phosphate buffer and extracted three times with EtOAc. The organic extracts were washed with brine and dried with sodium sulfate. Radial silica gel chromatography eluting with DCM containing 0 to 15% EtOAc afforded the title compound (4.1 mg) as oil.
後処理
- customThe bath was removed
- waitthe reaction was left
- additionAqueous 1 N HCl was added
- waitthe reaction was left
- stirringstirring for 20 min
- extractionextracted three times with EtOAc
- washThe organic extracts were washed with brine
- dry with materialdried with sodium sulfate
- washRadial silica gel chromatography eluting with DCM containing 0 to 15% EtOAc
出典と根拠
- ORDレコード
- ord-b23867537013472ebed78883b6eab118
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09273057B2
関連ノート
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