Hydrochloric Acid → Methyl Vanillate

반응식

[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

참가 물질

반응물 3

HCID 313Hydrochloric Acid

HCID 887Methanol

HCID 8468Vanillic Acid

생성물 1

HCID 19844Methyl Vanillate수율 91.5%

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록: ord-05457a0b469b492b972192d9954573fb
출처 데이터셋: uspto-grants-2010_06
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07745490B2

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