Methanol → Methyl Ferulate

HRID 987875

反応式

HRID 987875 の反応式
[OH:1][C:2]1[CH:12]=[CH:11][C:5](/[CH:6]=[CH:7]/[C:8]([OH:10])=[O:9])=[CH:4][C:3]=1[O:13][CH3:14].S(=O)(=O)(O)O.[CH3:20]O>>[OH:1][C:2]1[CH:12]=[CH:11][C:5](/[CH:6]=[CH:7]/[C:8]([O:10][CH3:20])=[O:9])=[CH:4][C:3]=1[O:13][CH3:14]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 445858Ferulic Acid

生成物 1

HCID 5357283Methyl Ferulate

実験手順

25 g (0.13 mol) of (E)-4-hydroxy-3-methoxycinnamic acid were dissolved in 180 ml of methanol and 5 ml of concentrated sulfuric acid was added. The solution was refluxed for 2 hours. Thereafter, the major part of the methanol (about 150 ml) was distilled off and the residue was poured onto 500 ml of ice water. The precipitated ester was filtered off with suction, washed in succession with cold water, with a little cold NaHCO3 solution and again with cold water and dried at 50° C. under reduced pressure from a water-jet pump. Chromatography over 250 g of silica gel using dichloromethane/diethyl ether (19:1) gave 21.78 g of methyl (E)-4-hydroxy-3-methoxycinnamate as a pale yellow oil.

後処理

  1. temperatureThe solution was refluxed for 2 hours
  2. distillationThereafter, the major part of the methanol (about 150 ml) was distilled off
  3. additionthe residue was poured onto 500 ml of ice water
  4. filtrationThe precipitated ester was filtered off with suction
  5. washwashed in succession with cold water, with a little cold NaHCO3 solution and again with cold water
  6. dry with materialdried at 50° C. under reduced pressure from a water-jet pump

出典と根拠

ORDレコード
ord-6b70f3881c9e482fb1b8369bd18ef924
出典データセット
uspto-grants-2003_10
特許番号
US06632909B2

関連ノート

読み込み中…