Water → (2-Methylpyridin-4-yl)methanol

HRID 279612

反応式

HRID 279612 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8](OC)=[O:9])[CH:5]=[CH:4][N:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>CCOCC>[OH:9][CH2:8][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([CH3:1])[CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 11542811Methyl 2-methylisonicotinateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 9942144(2-Methylpyridin-4-yl)methanol収率 38%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
5 °C

実験手順

A solution of methyl 2-methyl-pyridine-4-carboxylate (800 mg, 6 mmol) in ether (5 ml) was added to lithium aluminium hydride (340 mg, 9mmol) in ether (10 ml) cooled to 5° C. and the mixture stirred for 2 hours. Water was added, the mixture was filtered through diatomaceous earth and the pad was washed through with ethyl acetate. The filtrate was extracted with ethyl acetate and the combined extracts were washed with brine, dried (MgSO4) and the solvent removed by evaporation to give 4-hydroxymethyl-2-methylpyridine (240 mg, 38%) as a yellow oil.

後処理

  1. filtrationthe mixture was filtered through diatomaceous earth
  2. washthe pad was washed through with ethyl acetate
  3. extractionThe filtrate was extracted with ethyl acetate
  4. washthe combined extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. customthe solvent removed by evaporation

出典と根拠

ORDレコード
ord-b0a10f74ee6e4ac7b5572d06957e5e55
出典データセット
uspto-grants-2002_03
特許番号
US06362336B1

関連ノート

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