Methanol → Methyl 2-hydroxy-6-methoxybenzoate

HRID 892185

반응식

HRID 892185 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([OH:12])[C:8]=1[C:9]([OH:11])=[O:10].[CH3:13]O>S(=O)(=O)(O)O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([OH:12])[C:8]=1[C:9]([O:11][CH3:13])=[O:10]

참가 물질

4

반응물 2

HCID 887MethanolHCID 5915242-Hydroxy-6-methoxybenzoic acid

생성물 1

HCID 527092Methyl 2-hydroxy-6-methoxybenzoate

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A mixture of 6-methoxysalicylic acid (10.0 g, 59.5 mmol) in methanol (40 mL) and sulfuric acid (2 mL) is heated at reflux 48 h. Although some acid remains the reaction is concentrated to remove the methanol and partitioned between ethyl acetate and saturated sodium carbonate solution. The organic phase is separated and washed with sodium carbonate until no acid remains by TLC analysis. The organic phase is dried and concentrated to provide the title compound as a low melting solid.

후처리

  1. temperatureis heated
  2. temperatureat reflux 48 h
  3. concentrationis concentrated
  4. customto remove the methanol
  5. custompartitioned between ethyl acetate and saturated sodium carbonate solution
  6. customThe organic phase is separated
  7. washwashed with sodium carbonate until no acid
  8. customThe organic phase is dried
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-be9d3173ea9943d198c95c9532640032
출처 데이터셋
uspto-grants-2006_02
특허 번호
US07005440B1

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