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

HRID 349923

反応式

HRID 349923 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f629b2eadfef435bb5d41732fed7d2f2
出典データセット
uspto-grants-2007_02
特許番号
US07179823B1

関連ノート

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