Water → 2-Methoxy-6-methylpyridin-3-ol

HRID 416555

反応式

HRID 416555 の反応式
Cl[C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1.[CH3:10][O-:11].[Na+].CO.O>C(O)(=O)C>[CH3:10][O:11][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1

参加物

5

反応物 3

HCID 962WaterHCID 30157972-Chloro-6-methylpyridin-3-olHCID 23694274Sodium methanolate methanol

生成物 1

HCID 234638212-Methoxy-6-methylpyridin-3-ol収率 48.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

In metal sealed tube were added 2-chloro-3-hyroxy-6-methylpyridine (1-014-02) (22.91 g) and 28% sodium methoxide/methanol solution (120 mL) and the reaction mixture was reacted at 150° C. for 3 days. To the reaction mixture was added ice and water (100 mL) and the reaction mixture was neutralized with acetic acid, and evaporated completely. The residue was purified by silica gel column chromatography (chloroform) to give the desired 2-methoxy-3-hyroxy-6-methylpyridine (1-014-03) (10.44 g, 48.1%). Furthermore, the fraction contained the starting material was reacted in sealed tube again.

後処理

  1. customIn metal sealed tube
  2. customthe reaction mixture was reacted at 150° C. for 3 days
  3. customevaporated completely
  4. customThe residue was purified by silica gel column chromatography (chloroform)

出典と根拠

ORDレコード
ord-ef4cb71f106b46b9ad72c703118fd199
出典データセット
uspto-grants-2012_01
特許番号
US08088924B2

関連ノート

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