Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethyl Sulfide | HCID 1068 | — |
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 14403422 | HCID 14403422 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 14348395 | HCID 14348395 | 75% |
Reaction Steps
16 ml (0.22 mol) of dimethyl sulphide and 24.2 g (0.19 mol) of dimethyl sulphate are added to 30 ml of tert.-butanol and allowed to stand at 20° C. for 14 hours. A solution of 17 g (0.07 mol) of 1-chlorocyclopropyl 4-chlorophenylethyl ketone in 70 ml of tert.-butanol is first added dropwise to the reaction mixture with stirring and 22 g of potassium hydroxide powder are then introduced, while the temperature of the reaction mixture is kept at 20° to 30° C. The mixture is stirred at 30° C. for 3 hours more, then the dimethyl sulphide is removed under reduced pressure and the reaction mixture is then poured into 50 ml of a 1% aqueous hydrogen peroxide solution. The mixture is extracted with ethyl acetate. The organic phase is washed with water and concentrated by removing the solvent under reduced pressure after drying over sodium sulphate. In this manner, 13.4 g (75 % of theory) of 2-(1-chlorocyclopropyl)-2-(4-chlorophenylethyl)-oxirane are obtained in the form of an oily product, which is reacted further without additional purification. ##STR64##
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04925865 |
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| Source dataset | uspto-grants-1990_05 |
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| ORD ID | ord-689d192d09304321b173e7d6ef3916e6 |
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| Source note | uspto-grants-1990_05 |
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