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

HRID 2378710노트

반응식

HRID 2378710 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-88d46f27265349149ee1bd6aa3e214e1
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07470717B2

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