Urea → 3-Iodophthalic acid

HRID 21110

反応式

HRID 21110 の反応式
N[C:2]1[CH:10]=[CH:9][CH:8]=[C:4]([C:5]([OH:7])=[O:6])[C:3]=1[C:11]([OH:13])=[O:12].[N+]([O-])([O-])=O.[Na+].[I-:19].[K+].NC(N)=O.S([O-])([O-])(=O)=S.[Na+].[Na+]>Cl>[I:19][C:2]1[CH:10]=[CH:9][CH:8]=[C:4]([C:5]([OH:7])=[O:6])[C:3]=1[C:11]([OH:13])=[O:12]

参加物

7

反応物 5

HCID 1176UreaHCID 4875Potassium IodideHCID 24268Sodium NitrateHCID 24477Sodium ThiosulfateHCID 794903-Aminophthalic acid

生成物 1

HCID 2382313-Iodophthalic acid収率 62%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

3-Aminophthalic acid (5.00 g, 27.6 mmol) was dissolved in 8.4 mol/L hydrochloric acid (60 mL), and the solution was added with an aqueous solution (10 mL) of sodium nitrate (2.0 g, 29 mmol) by drops under ice-cooling for 20 minutes, followed by stirring at the same temperature for 3 hours. Then, an aqueous solution (10 mL), in which potassium iodide (6.9 g, 41 mmol) and urea (291 mg) were dissolved, is added by drops to the mixture, followed by stirring at room temperature for 20 hours. The reaction mixture was added with 10% aqueous sodium thiosulfate solution and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was washed with chloroform to obtain 3-iodophthalic acid (5.0 g, yield 62%).

後処理

  1. temperaturecooling for 20 minutes
  2. additionis added by drops to the mixture
  3. stirringby stirring at room temperature for 20 hours
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. washthe residue was washed with chloroform

出典と根拠

ORDレコード
ord-e0e207c6299d4555b2027fedb6fcecfc
出典データセット
uspto-grants-2010_06
特許番号
US07745641B2

関連ノート

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