Hydrogen Peroxide → Monoperoxyphthalic acid

HRID 719846

반응식

HRID 719846 반응식
C([O-])([O-])=O.[Na+].[Na+].[OH:7][OH:8].[C:9]1(=[O:19])[O:14][C:12](=[O:13])[C:11]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:10]12.OS(O)(=O)=O>O>[CH:17]1[CH:18]=[C:10]([C:9]([OH:14])=[O:19])[C:11]([C:12]([O:7][OH:8])=[O:13])=[CH:15][CH:16]=1

참가 물질

6

반응물 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 6811Phthalic AnhydrideHCID 10340Sodium Carbonate

생성물 1

HCID 75329Monoperoxyphthalic acid수율 76.9%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Deionized water (125 ml), Na2CO3 (31.0 g, 0.25 mol) and 35% H2O2 (29.15 g, 0.3 mol) are successively charged in a 500 ml four-neck flask, and the mixture was stirred in a dry ice-methanol bath at −5° C.–0° C. Thereto was added phthalic anhydride (37.0 g, 0.25 mol) and the mixture was stirred for 30 min. The bath was removed, ethyl acetate (100 ml) was added to the mixture, and the reaction system was neutralized in a solution obtained by diluting 98% H2SO4 (15 ml) with deionized water (50 ml). After partitioning, the aqueous layer was extracted with ethyl acetate (60 ml). The obtained organic layer (0.64 g) was taken up and saturated NaI-IPA (isopropyl alcohol) solution (5 ml) and 10% acetic acid-IPA solution (20 ml) were added thereto. The mixture was boiled for 5 min. It was titrated with 0.1N aqueous sodium thiosulfate solution. As a result, mono-perphthalic acid was present in 33.5 g and the yield was 76.9%.

후처리

  1. stirringthe mixture was stirred for 30 min
  2. customThe bath was removed
  3. additionethyl acetate (100 ml) was added to the mixture
  4. customobtained
  5. customAfter partitioning
  6. extractionthe aqueous layer was extracted with ethyl acetate (60 ml)
  7. additionsaturated NaI-IPA (isopropyl alcohol) solution (5 ml) and 10% acetic acid-IPA solution (20 ml) were added

출처 및 근거

ORD 기록
ord-ad9fdcc6fe6045d58fb91747ed8a1665
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07132560B2

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