Hydrochloric Acid → Methyl Vanillate

反応式

[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[O:11][CH3:12].Cl.[CH3:14]O>>[CH3:14][O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([OH:1])=[C:3]([O:11][CH3:12])[CH:4]=1

参加物

反応物 3

HCID 313Hydrochloric Acid

HCID 887Methanol

HCID 8468Vanillic Acid

生成物 1

HCID 19844Methyl Vanillate収率 91.5%

実験手順

A solution of 4-hydroxy-3methoxy benzoic acid (7.2 g) in methanol (150 ml) was refluxed in presence of concentrated hydrochloric acid (0.5 ml) for 12 hrs. After concentrating under reduced pressure, the residue was dissolved in ethyl acetate (200 ml) and washed with water (50 ml) 10% sodium bicarbonate solution (2×50 ml), water (50 ml) and dried over anhydrous magnesium sulfate. Removal of the solvent under reduced pressure provided 7.25 g of 4-hydroxy-3-methoxy benzoic acid methyl ester. (Yield=91.5%).

後処理

concentrationAfter concentrating under reduced pressure
dissolutionthe residue was dissolved in ethyl acetate (200 ml)
washwashed with water (50 ml) 10% sodium bicarbonate solution (2×50 ml), water (50 ml)
dry with materialdried over anhydrous magnesium sulfate
customRemoval of the solvent under reduced pressure

出典と根拠

ORDレコード: ord-05457a0b469b492b972192d9954573fb
出典データセット: uspto-grants-2010_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07745490B2

反応ノート

読み込み中…

参加物