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Hydrogen Peroxide → 2-(2,4-Dichlorophenylethenyl)-2-(1-propylmercaptocyclopropyl) oxirane

HRID 1089897
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HRID 1089897 반응식
CSC.S([O:9][CH3:10])(OC)(=O)=O.[CH2:11]([S:14][C:15]1([C:18]([CH:20]=[CH:21][C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=2[Cl:29])=O)[CH2:17][CH2:16]1)[CH2:12][CH3:13].[OH-].[K+].OO>C(O)(C)(C)C>[Cl:29][C:23]1[CH:24]=[C:25]([Cl:28])[CH:26]=[CH:27][C:22]=1[CH:21]=[CH:20][C:18]1([C:15]2([S:14][CH2:11][CH2:12][CH3:13])[CH2:16][CH2:17]2)[CH2:10][O:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 784Hydrogen PeroxideHCID 1068Dimethyl Sulfide2회HCID 6497Dimethyl SulfateHCID 14797Potassium HydroxideHCID 54332237HCID 54332237, 화합물

생성물 1

HCID 540874812-(2,4-Dichlorophenylethenyl)-2-(1-propylmercaptocyclopropyl) oxirane수율 91%

시약·촉매·용매

1
HCID 6386tert-Butanol용매2회

실험 절차

30 ml (0.41 mol) of dimethyl sulphide and 43.5 g (0.35 mol) of dimethyl sulphate are added to 60 ml of tert.-butanol and allowed to stand at room temperature for 14 hours. A solution of 40 g (0.13 mol) of 2,4-dichlorophenyl-ethenyl 1-propylmercaptocyclopropyl ketone in 120 ml of tert.-butanol is initially added dropwise to the reaction mixture with stirring and then 39.1 g of potassium hydroxide powder is introduced, the temperature of the reaction mixture being held at 20° to 30° C. The mixture is stirred for a further 3 hours at 30° C., then the dimethyl sulphide is stripped off under reduced pressure and the reaction mixture is then poured into 70 ml of a 1% strength aqueous hydrogen peroxide solution. The mixture is extracted with ethyl acetate. The organic phase is washed using water and concentrated by stripping off the solvent under reduced pressure after drying over sodium sulphate. In this manner, 38.2 g (91% of theory) of 2-(2,4-dichlorophenylethenyl)-2-(1-propylmercaptocyclopropyl)-oxirane are obtained in the form of an oily product, which is further reacted without additional purification. ##STR77##

후처리

  1. custombeing held at 20° to 30° C
  2. stirringThe mixture is stirred for a further 3 hours at 30° C.
  3. extractionThe mixture is extracted with ethyl acetate
  4. washThe organic phase is washed
  5. concentrationconcentrated
  6. dry with materialafter drying over sodium sulphate

출처 및 근거

ORD 기록
ord-7c6d932fff0a400bb05521e9cac4cc82
출처 데이터셋
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05079374

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