Sodium sulfate decahydrate → (1-ethyl-1H-pyrazol-4-yl)methanol

HRID 2221660노트

반응식

HRID 2221660 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:9]1[CH:13]=[C:12]([C:14](OCC)=[O:15])[CH:11]=[N:10]1)[CH3:8].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH2:7]([N:9]1[CH:13]=[C:12]([CH2:14][OH:15])[CH:11]=[N:10]1)[CH3:8]

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 17862887HCID 17862887, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 4711794(1-ethyl-1H-pyrazol-4-yl)methanol수율 78%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Lithium aluminum hydride (7.19 g) was suspended in tetrahydrofuran (400 mL). To the obtained mixture were added a solution (100 mL) of ethyl 1-ethyl-1H-pyrazole-4-carboxylate (29.00 g) in tetrahydrofuran on an ice bath with stirring. After stirring the reaction mixture at room temperature for 1.5 hrs, sodium sulfate decahydrate (80 g) was added by small portions on an ice bath with stirring, and the mixture was further stirred at room temperature for 16 hrs. The solid was filtered, and the filtrate was concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give (1-ethyl-1H-pyrazol-4-yl)methanol as a colorless oil (16.85 g, yield 78%) from a fraction eluted with ethyl acetate-methanol (1:0 to 49:1, v/v).

후처리

  1. stirringAfter stirring the reaction mixture at room temperature for 1.5 hrs
  2. stirringwith stirring
  3. stirringthe mixture was further stirred at room temperature for 16 hrs
  4. filtrationThe solid was filtered
  5. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0c204cfa04594a2b8504ffe83a411fad
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07368578B2

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