Hydrogen Peroxide → 3-Sulphoperoxybenzoic acid

HRID 485216

반응식

HRID 485216 반응식
[S:1]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])([OH:4])(=[O:3])=[O:2].[OH:14]O>ClCCl.S(=O)(=O)(O)O>[S:1]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([O:10][OH:14])=[O:9])([OH:4])(=[O:3])=[O:2]

참가 물질

5

반응물 2

HCID 784Hydrogen PeroxideHCID 8477Benzoic acid, 3-sulfo-

생성물 1

HCID 98158233-Sulphoperoxybenzoic acid수율 64.2%

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 6344Dichloromethane용매

반응 조건

온도
42 °C

실험 절차

To a suspension of 3-sulphobenzoic acid (5 g, 2.5×10-2 moles) in dichloromethane (60 ml) containing a trace of sulphuric acid (5×10-5 moles) was slowly added hydrogen peroxide (3 g; 85%). The suspension was boiled under reflux (42° C.) for 1 hour after which it was cooled to room temperature, the dichloromethane was decanted off and the residue treated with saturated aqueous magnesium nitrate (25 ml). The resultant precipitate was filtered off, dried over phosphorous pentoxide under vacuum to yield the magnesium salt of 3-sulphoperoxybenzoic acid (3.5 g; 5.31% Avox as O; Magnesium content of 4.7%) compared with a theoretical yield of 5.67 g. The IR spectrum was again substantially the same as for the other preparations.

후처리

  1. temperaturewas cooled to room temperature
  2. customthe dichloromethane was decanted off
  3. additionthe residue treated with saturated aqueous magnesium nitrate (25 ml)
  4. filtrationThe resultant precipitate was filtered off
  5. dry with materialdried over phosphorous pentoxide under vacuum

출처 및 근거

ORD 기록
ord-0cff83a548e745d9ac7dc42b94745dbf
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536313

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