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

HRID 1639759ノート

反応式

HRID 1639759 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-767e125884e64b6aad13f682585799fe
出典データセット
uspto-grants-2012_02
特許番号
US08110585B2

反応ノート

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