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

HRID 508390

반응식

HRID 508390 반응식
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]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 962Water2회HCID 10340Sodium CarbonateHCID 2229632-Bromo-4,5-dimethoxybenzoic acid

생성물 1

HCID 115646502-Hydroxy-4,5-dimethoxybenzoic acid수율 99.3%

시약·촉매·용매 3

HCID 24462Copper Sulfate촉매HCID 24463Copper sulfate pentahydrate촉매HCID 1049Pyridine용매

반응 조건

온도
80 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-a7cb3dd4c9b4463dafab59d1590e826e
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096511B2

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