Sodium sulfate decahydrate → (1H-Indazol-3-yl)-N,N-dimethylmethanamine

HRID 2075427ノート

反応式

HRID 2075427 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][N:8]([CH3:20])[C:9]([C:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[NH:13][N:12]=1)=O.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH3:20][N:8]([CH2:9][C:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[NH:13][N:12]=1)[CH3:7]

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 20816326N,N-Dimethyl-1H-indazole-3-carboxamideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 178483331(1H-Indazol-3-yl)-N,N-dimethylmethanamine収率 76.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Lithium aluminum hydride (13.7 g, 36.1 mmol) was suspended in THF (500 mL), and the suspension was added with a solution of N,N-dimethyl-1H-indazole-3-carboxamide obtained in Step 1 (34.2 g, 181 mmol) in THF (250 mL), followed by stirring at room temperature under the flow of nitrogen gas for 30 minutes. The reaction mixture was mixed with sodium sulfate decahydrate, was stirred for further 1 hour and was filtered through Celite. The solvent was evaporated under reduced pressure to obtain 3-dimethylaminomethyl-1H-indazole (24.2 g, 76%).

後処理

  1. stirringwas stirred for further 1 hour
  2. filtrationwas filtered through Celite
  3. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-8acd899441a34927b8dade6c100ef8f8
出典データセット
uspto-grants-2011_04
特許番号
US07919517B2

反応ノート

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