Hexane → [3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-4-yl]methanol

HRID 349923

반응식

HRID 349923 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[C:12]([C:13](OCC)=[O:14])=[CH:11][N:10]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)[N:9]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].CCCCCC>O1CCCC1>[CH3:7][C:8]1[C:12]([CH2:13][OH:14])=[CH:11][N:10]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)[N:9]=1

참가 물질

6

반응물 4

HCID 8058HexaneHCID 62649Sodium sulfate decahydrateHCID 9877977ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 23076503[3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-4-yl]methanol수율 92.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Lithium aluminium hydride (1.93 g) was added to a solution of ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylate (15.00 g) in tetrahydrofuran (150 ml) at 0° C., and the mixture was stirred at room temperature for one hour. Sodium sulfate decahydrate (21.03 g) and hexane (100 ml) were added to the reaction mixture, and the mixture was stirred at room temperature for one hour. After the precipitate was removed by filtration, the filtrate was concentrated. The crystals obtained were collected by filtration to yield [3-methyl-1-(2-pyridyl)-1H-pyrazol-4-yl]methanol (11.38 g). This was recrystallized from acetone-hexane. Melting point: 116–117° C.

후처리

  1. stirringthe mixture was stirred at room temperature for one hour
  2. customAfter the precipitate was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. customThe crystals obtained
  5. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-f629b2eadfef435bb5d41732fed7d2f2
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179823B1

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