Hydrogen Peroxide → 3-Sulphoperoxybenzoic acid

HRID 485216

反応式

HRID 485216 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 98158233-Sulphoperoxybenzoic acid収率 64.2%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 6344Dichloromethane溶媒

反応条件

温度
42 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0cff83a548e745d9ac7dc42b94745dbf
出典データセット
uspto-grants-1985_08
特許番号
US04536313

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