Dopac → Methyl 3,4-dihydroxyphenylacetate

HRID 582047

反応式

HRID 582047 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([OH:12])=[O:11])[CH:5]=[CH:6][C:7]=1[OH:8].S(=O)(=O)(O)O.[CH3:18]O>>[OH:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([O:12][CH3:18])=[O:11])[CH:5]=[CH:6][C:7]=1[OH:8]

参加物

4

反応物 3

HCID 547DopacHCID 887MethanolHCID 1118Sulfuric Acid

生成物 1

HCID 11008556Methyl 3,4-dihydroxyphenylacetate

実験手順

A mixture of 3,4-dihydroxyphenylacetic acid (10.0 g) and concentrated sulphuric acid (0.5 ml ) in methanol (70 ml) was heated under reflux for 16 hours. The mixture was concentrated, water was added and the mixture was neutralised to pH7 using sodium carbonate. The cloudy solution obtained was extracted with dichloromethane (200 ml), dried (Na2SO4) and evaporated to give a yellow gum (7.64 g). LRMS m/z=183(m+1)+.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. concentrationThe mixture was concentrated
  4. additionwater was added
  5. customThe cloudy solution obtained
  6. extractionwas extracted with dichloromethane (200 ml)
  7. dry with materialdried (Na2SO4)
  8. customevaporated

出典と根拠

ORDレコード
ord-eccd76d2b243402faaa07ef69d3c5c89
出典データセット
uspto-grants-1999_07
特許番号
US05922747

関連ノート

読み込み中…