Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Carbon Disulfide | HCID 6348 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | cis-1,2-Dichloroethylene | HCID 643833 | — |
| Edukt | Methanesulfonylacetic acid methyl ester | HCID 2759918 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 21245351 | HCID 21245351 | 83% |
Reaktionsschritte
To a mixture of 15.2 g of methyl methylsulfonylacetate, 7.6 g of carbon disulfide and 200 ml of dimethylformamide, 14.0 g of potassium hydroxide was added under ice-cooling. The resultant mixture was stirred for 3 hours. Thereafter, 9.7 g of cis-1,2-dichloroethylene was added, followed by stirring at 80° C. for 4 hours. After cooling the reaction mixture, chloroform and water were added and the resulting organic layer was separated. Upon removal of the solvent by distillation under reduced pressure, 20.9 g of the title compound was obtained as pale yellow crystals. Upon recrystallization from a mixed solvent of chloroform and n-hexane, they turned to white crystals. Melting point: 166°-168° C. (decomposed).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04822814 |
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| Quelldatensatz | uspto-grants-1989_04 |
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| ORD ID | ord-31daf46e689444fab9094eaf7c6d49e2 |
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| Quellennotiz | uspto-grants-1989_04 |
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