Hydrochloric Acid → 2-Hydroxy-4,5-dimethoxybenzoic acid

HRID 508390

反応式

HRID 508390 の反応式
O.Br[C:3]1[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6].C(=O)([O-])[O-:17].[Na+].[Na+].Cl>S([O-])([O-])(=O)=O.[Cu+2].O.O.O.O.O.S([O-])([O-])(=O)=O.[Cu+2].N1C=CC=CC=1>[OH:17][C:3]1[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 962Water2 回HCID 10340Sodium CarbonateHCID 2229632-Bromo-4,5-dimethoxybenzoic acid

生成物 1

HCID 115646502-Hydroxy-4,5-dimethoxybenzoic acid収率 99.3%

試薬・触媒・溶媒 3

HCID 24462Copper Sulfate触媒HCID 24463Copper sulfate pentahydrate触媒HCID 1049Pyridine溶媒

反応条件

温度
80 °C

実験手順

Water (80 mL) was added to the crude crystals of 2-bromo-4,5-dimethoxybenzoic acid produced in Example 1 (20.0 g) and sodium carbonate (10.1 g). The resultant mixture was stirred under heating at 80° C., and a copper sulfate solution prepared from copper sulfate pentahydrate (1.91 g), water (20 mL), and pyridine (3.1 mL) was added to the mixture. The resultant mixture was further heated and stirred at 90 to 100° C. for one hour. The mixture was cooled to 50° C., and concentrated hydrochloric acid (16.0 g) was added dropwise thereto. After cooling of the mixture, the precipitated crystals were filtrated, and then dried under reduced pressure, to thereby produce crude crystals of 2-hydroxy-4,5-dimethoxybenzoic acid (15.08 g) (yield: 99.3%).

後処理

  1. additionwas added to the mixture
  2. temperatureThe mixture was cooled to 50° C.
  3. temperatureAfter cooling of the mixture
  4. filtrationthe precipitated crystals were filtrated
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-a7cb3dd4c9b4463dafab59d1590e826e
出典データセット
uspto-grants-2015_08
特許番号
US09096511B2

関連ノート

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