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Citric Acid → 2,3-Dihydroxybenzoic Acid

HRID 2413520
ノート
印刷プレビュー

反応式

HRID 2413520 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 311Citric AcidHCID 338Salicylic AcidHCID 14797Potassium HydroxideHCID 135865461,4-Dihydropyridine-3-carboxamide2 回HCID 178503009HCID 178503009、化合物

生成物 1

HCID 192,3-Dihydroxybenzoic Acid収率 5,963%

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-2bb416cfdfb147dc81f1cd4adc369c33
出典データセット
uspto-grants-1988_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04718994

反応ノート

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