HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl[(trichloromethyl)sulfanyl]carbamyl fluoride → 5,5-Dimethyl-2-ethylimino-4-[[O-[N-methyl-N-(trichloromethanesulfenyl)carbamoyl]oximino]]-1,3-dithiolane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl[(trichloromethyl)sulfanyl]carbamyl fluoride | HCID 12836648 | — |
| Edukt | 5,5-Dimethyl-2-ethylimino-4-oximino-1,3-dithiolane | HCID 85976754 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 5,5-Dimethyl-2-ethylimino-4-[[O-[N-methyl-N-(trichloromethanesulfenyl)carbamoyl]oximino]]-1,3-dithiolane | HCID 54312720 | 57,4% |
Reaktionsschritte
To a solution of 3.5 grams (0.017m) of 5,5-dimethyl-2-ethylimino-4-oximino-1,3-dithiolane (XXIII) and 3.84 grams (0.017m) of N-methyl-N-trichloromethanesulfenyl carbamoyl fluoride in 75 ml of dioxane, was added dropwise with stirring 1.71 grams (0.017m) of triethylamine. After allowing the reaction mixture to stand at room temperature for 16 hours it was diluted with 250 ml of cold water and was extracted in ethylacetate. The organic extract was washed with water, dried over magnesium sulfate and concentrated under reduced pressure to a residual oil which crystallized on the addition of isopropyl ether and hexane, to afford 4.0 grams of a white solid. m.p. 69°-71° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04156731 |
| Quelldatensatz | uspto-grants-1979_05 |
| ORD ID | ord-e38e112a826a47ed8f9ce78c31a4ee39 |
| Quellennotiz | uspto-grants-1979_05 |