Water → (2-Methylpyridin-3-yl)methanol

HRID 856704

反応式

HRID 856704 の反応式
[H-].[Li+].[Al+3].[H-].[H-].[H-].[CH3:7][C:8]1[N:17]=[CH:16][CH:15]=[CH:14][C:9]=1[C:10](OC)=[O:11].O.[OH-].[Na+]>C1COCC1>[CH3:7][C:8]1[C:9]([CH2:10][OH:11])=[CH:14][CH:15]=[CH:16][N:17]=1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 7015327Methyl 2-methylnicotinateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 302564(2-Methylpyridin-3-yl)methanol収率 70.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of aluminum lithium hydride (2.0 g) in THF (160 ml) was added dropwise a solution of methyl 2-methylnicotinate (8.0 g) in THF (80 ml) at 0° C. The mixture was stirred for 2 hours at room temperature, and water (8.0 ml), 15% aqueous solution of sodium hydroxide (8.0 ml) and water (24.0 ml) were sequentially added to the mixture at 0° C. The mixture was filtered with Celite, and washed with methanol. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to give (2-methyl-3-pyridinyl)methanol (4.6 g).

後処理

  1. filtrationThe mixture was filtered with Celite
  2. washwashed with methanol
  3. customThe solvent was removed under reduced pressure
  4. customthe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-2a9563f0cf564642a63a6036f515f015
出典データセット
uspto-grants-2007_08
特許番号
US07262185B2

関連ノート

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