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

HRID 416555

반응식

HRID 416555 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 234638212-Methoxy-6-methylpyridin-3-ol수율 48.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ef4cb71f106b46b9ad72c703118fd199
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088924B2

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