Sulfuric Acid → 5-Nitrobenzene-1,2,3-tricarboxylic acid

HRID 1389699

반응식

HRID 1389699 반응식
[C:1]1([C:13]([OH:15])=[O:14])[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([OH:9])=[O:8])[C:2]=1[C:10]([OH:12])=[O:11].S(=O)(=O)(O)O.[N+:21]([O-])([O-:23])=[O:22].[K+]>O>[N+:21]([C:5]1[CH:6]=[C:1]([C:13]([OH:15])=[O:14])[C:2]([C:10]([OH:12])=[O:11])=[C:3]([C:7]([OH:9])=[O:8])[CH:4]=1)([O-:23])=[O:22]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 112881,2,3-Benzenetricarboxylic acidHCID 24434Potassium Nitrate

생성물 1

HCID 144348595-Nitrobenzene-1,2,3-tricarboxylic acid

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a stirred mixture of 125 g. of 1,2,3-benzenetricarboxylic acid and 900 ml. of concentrated sulfuric acid at 60°-70° C. is added, gradually over a 2 hour period, 312 g. of potassium nitrate. The mixture is heated at 135°-140° C. for 16 hours, cooled and treated with ice and water. Some solid is seprated out and is dissolved in water. The entire aqueous mixture is extracted with ether, the extract is washed with water and dried over magnesium sulfate. The ether is concentrated to a small volume, and petroleum ether is added to precipitate a white solid. The solid is collected and dried to give 76.5 g. of the product of the Example.

후처리

  1. additionTo a stirred mixture of 125 g
  2. temperatureThe mixture is heated at 135°-140° C. for 16 hours
  3. temperaturecooled
  4. extractionThe entire aqueous mixture is extracted with ether
  5. washthe extract is washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationThe ether is concentrated to a small volume, and petroleum ether
  8. additionis added
  9. customto precipitate a white solid
  10. customThe solid is collected
  11. customdried
  12. customto give 76.5 g

출처 및 근거

ORD 기록
ord-f6e7e0af7c074fe39bc516d750ab9f2f
출처 데이터셋
uspto-grants-1981_01
특허 번호
US04245119

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