Methanol → alpha-Methyl-2-pyridinemethanol

HRID 230778ノート

反応式

HRID 230778 の反応式
CO.[N:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9](=[O:11])[CH3:10].[BH4-].[Na+]>O>[N:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]([OH:11])[CH3:10]

参加物

5

反応物 3

HCID 887MethanolHCID 142862-AcetylpyridineHCID 4311764Sodium borohydride

生成物 1

HCID 86784alpha-Methyl-2-pyridinemethanol収率 88.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A methanol solution (100 mL) of 1-pyridin-2-ylethanone (10.0 g) was cooled to 0° C., sodium borohydride (6.2 g) was added thereto and stirred at that temperature for 4 hours. Then water was added to the reaction solution, and the organic solvent was evaporated off under reduced pressure. The resulting residue was extracted with ethyl acetate. The organic layer was dried with anhydrous magnesium sulfate, and the solvent was evaporated off under reduced pressure. The resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=4/1 to 3/2) to obtain the entitled compound (9.0 g).

後処理

  1. customthe organic solvent was evaporated off under reduced pressure
  2. extractionThe resulting residue was extracted with ethyl acetate
  3. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  4. customthe solvent was evaporated off under reduced pressure
  5. customThe resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=4/1 to 3/2)

出典と根拠

ORDレコード
ord-971f629345c146689a8e5e3f7eccb98a
出典データセット
uspto-grants-2009_07
特許番号
US07566781B2

反応ノート

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