Methanol → 3-Methoxy-2-methylpyridine

HRID 128612ノート

反応式

HRID 128612 の反応式
[CH3:1][O-].[Na+].CO.[OH:6][C:7]1[C:8]([CH3:13])=[N:9][CH:10]=[CH:11][CH:12]=1>CN(C=O)C>[CH3:1][O:6][C:7]1[C:8]([CH3:13])=[N:9][CH:10]=[CH:11][CH:12]=1

参加物

5

反応物 3

HCID 887MethanolHCID 707192-Methylpyridin-3-olHCID 10942334Sodium Methoxide

生成物 1

HCID 30152703-Methoxy-2-methylpyridine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of sodium methoxide (prepared from sodium metal) (10.2 g) and methanol (175 ml), 3-hydroxy-2-methylpyridine (43.0 g) phenyltrimethylammonium chloride (81.9 g) and DMF (400 ml) was boiled under reflux with stirring for 5 hours under nitrogen. The mixture was filtered and distilled. The fraction boiling at 167°-195° C. was collected and purified by flash chromatography on silica using dichloromethane and then IMS as the mobile phase to give 3-methoxy-2-methylpyridine which was used without further purification.

後処理

  1. temperatureunder reflux
  2. filtrationThe mixture was filtered
  3. distillationdistilled
  4. customThe fraction boiling at 167°-195° C. was collected
  5. custompurified by flash chromatography on silica

出典と根拠

ORDレコード
ord-9e78cd18ee884424b76f8b82d9556edd
出典データセット
uspto-grants-1995_11
特許番号
US05464781

反応ノート

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