Protocatechuic Acid → Methyl 3,4-Dihydroxybenzoate

HRID 19984

反応式

HRID 19984 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[OH:11])[C:5]([OH:7])=[O:6].Cl.[CH3:13]O>>[CH3:13][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][C:10]([OH:11])=[C:2]([OH:1])[CH:3]=1

参加物

4

反応物 3

HCID 72Protocatechuic AcidHCID 313Hydrochloric AcidHCID 887Methanol

生成物 1

HCID 287064Methyl 3,4-Dihydroxybenzoate収率 86.5%

実験手順

A solution of 3,4-dihydroxy benzoic acid (2.8 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 (150 ml) and washed with water (50 ml) 10% sodium bicarbonate solution (50 ml), brine solution (50 ml) and dried over anhydrous magnesium sulfate. Removal of the solvent under reduced pressure provided 2.64 g of 3,4-dihydroxybenzoic acid methyl ester. (Yield 86.5%).

後処理

  1. concentrationAfter concentrating under reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate (150 ml)
  3. washwashed with water (50 ml) 10% sodium bicarbonate solution (50 ml), brine solution (50 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customRemoval of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-10c90eac3e5d4cd08e4480474dc581bb
出典データセット
uspto-grants-2010_06
特許番号
US07745490B2

関連ノート

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