Sodium sulfate decahydrate → [3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol

HRID 2221653ノート

反応式

HRID 2221653 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH:7]([NH:9][C:10]1[C:14]([C:15](OCC)=[O:16])=[CH:13][N:12]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:11]=1)=O.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:7][NH:9][C:10]1[C:14]([CH2:15][OH:16])=[CH:13][N:12]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:11]=1

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23076448ethyl 3-(formylamino)-1-phenyl-1H-pyrazole-4-carboxylate

生成物 1

HCID 69217492[3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol収率 96%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

Lithium aluminum hydride (7.50 g) was added to tetrahydrofuran (200 mL) under ice-cooling. To the obtained mixture was added dropwise a solution (100 mL) of ethyl 3-(formylamino)-1-phenyl-1H-pyrazole-4-carboxylate (20.50 g) in tetrahydrofuran, and the mixture was heated under reflux for 1.5 hrs. To the obtained mixture was added small portions of sodium sulfate decahydrate (50 g) on an ice bath, and the mixture was stirred for 2 hrs. while adding tetrahydrofuran (50 mL) as appropriate to allow stirring. Solids were filtered off and the filtrate was concentrated to give [3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol as a colorless oil (15.42 g, yield 96%).

後処理

  1. temperaturecooling
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 1.5 hrs
  4. stirringto allow stirring
  5. filtrationSolids were filtered off
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-e787ff7a19494444a9d55a1cf4656842
出典データセット
uspto-grants-2008_05
特許番号
US07368578B2

反応ノート

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