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Citric Acid → 2,3-Dihydroxybenzoic Acid

HRID 2413520
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HRID 2413520 반응식
C(O)(=O)CC(CC(O)=O)(C(O)=O)O.[OH-].[K+].C(N)(=O)C1CC=CNC=1.[CH3:25][O:26]S([O-])(=O)=O.CC1C=CC=C2C=1N=C1C(C=CC=C1)=[NH+]2.[C:46]([OH:55])(=[O:54])[C:47]1[C:48](=C[CH:51]=[CH:52][CH:53]=1)[OH:49]>>[OH:49][C:48]1[C:25]([OH:26])=[CH:51][CH:52]=[CH:53][C:47]=1[C:46]([OH:55])=[O:54]
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참가 물질

6

반응물 5

HCID 311Citric AcidHCID 338Salicylic AcidHCID 14797Potassium HydroxideHCID 135865461,4-Dihydropyridine-3-carboxamide2회HCID 178503009HCID 178503009, 화합물

생성물 1

HCID 192,3-Dihydroxybenzoic Acid수율 5,963%

실험 절차

17 l of a 0.006M solution of citric acid are poured into a reactor and pH is brought to 4.5 by means of caustic potash, whereafter 17 g of cellulose modified with 1,4-dihydronicotinamide with the content of 0.2 mmol/g of dihydronicotinamide groups and 0.03 g of 9-methylphenazinium methylsulphate are added thereto and allowed to stand for 3 hours. Then 1.1 g of salicylic acid is added and the mixture is vigorously stirred for additional 3 hours. Cellulose modified 1,4-dihydronicotinamide is filtered off, the solution is evaporated to 100 ml and extracted with chloroform. The resulting extract is evaporated to 50 ml and cooled. The formed precipitate is crystallized with a mixture consisting of water and ethanol in the ratio of 1:1 to give 0.9 g of 2,3-dihydroxybenzoic acid (82% as calculated for the starting compound) having its melting point of 203°-204° C. Composition, in %, is as follows:

후처리

  1. additionare added
  2. filtrationis filtered off
  3. customthe solution is evaporated to 100 ml
  4. extractionextracted with chloroform
  5. extractionThe resulting extract
  6. customis evaporated to 50 ml
  7. temperaturecooled
  8. customThe formed precipitate is crystallized with a mixture

출처 및 근거

ORD 기록
ord-2bb416cfdfb147dc81f1cd4adc369c33
출처 데이터셋
uspto-grants-1988_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04718994

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