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

HRID 2221653노트

반응식

HRID 2221653 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-e787ff7a19494444a9d55a1cf4656842
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07368578B2

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