Sodium sulfate decahydrate → trans-1-[2-(2-Methylpyrazolo[1,5-a]pyridin-4-yl)cyclopropyl]methanamine

HRID 1639759노트

반응식

HRID 1639759 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[CH:22]=[C:11]2[C:12]([C@@H:16]3[CH2:18][C@H:17]3[CH:19]=[N:20]O)=[CH:13][CH:14]=[CH:15][N:10]2[N:9]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:7][C:8]1[CH:22]=[C:11]2[C:12]([C@@H:16]3[CH2:18][C@H:17]3[CH2:19][NH2:20])=[CH:13][CH:14]=[CH:15][N:10]2[N:9]=1

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 86641923trans-2-(2-Methylpyrazolo[1,5-a]pyridin-4-yl)cyclopropanecarbaldehyde oxime

생성물 1

HCID 59334541trans-1-[2-(2-Methylpyrazolo[1,5-a]pyridin-4-yl)cyclopropyl]methanamine수율 89%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of lithium aluminum hydride (1.18 g, 31.0 mmol) in tetrahydrofuran (70 mL) was added a solution of trans-2-(2-methylpyrazolo[1,5-a]pyridin-4-yl)cyclopropanecarbaldehyde oxime (1.67 g, 7.76 mmol) in tetrahydrofuran (8 mL) at room temperature, and the mixture was stirred at room temperature for 1.5 hr. Sodium sulfate decahydrate (17 g) was added under ice-cooling, and the mixture was filtered through celite. The filtrate was concentrated under reduced pressure to give the title compound (1.39 g, yield 89%).

후처리

  1. temperaturecooling
  2. filtrationthe mixture was filtered through celite
  3. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-767e125884e64b6aad13f682585799fe
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110585B2

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