Methanol → Methyl 2-hydroxy-6-methoxybenzoate

HRID 2117237

反応式

HRID 2117237 の反応式
[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]

参加物

4

反応物 2

HCID 887MethanolHCID 5915242-Hydroxy-6-methoxybenzoic acid

生成物 1

HCID 527092Methyl 2-hydroxy-6-methoxybenzoate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-29f75c0222e14271b3c012ee379abcbf
出典データセット
uspto-grants-2008_10
特許番号
USRE040558E1

関連ノート

読み込み中…