HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trichloromethanesulfenyl chloride → 5-Chloro 3-(2,4,6-trimethylphenyl)1,2,4-thiadiazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trichloromethanesulfenyl chloride | HCID 11666 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Mesitylformamidin | HCID 18788461 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 5-Chloro 3-(2,4,6-trimethylphenyl)1,2,4-thiadiazole | HCID 18788458 | 99,1% |
Reaktionsschritte
2.2 g of trichloromethanesulfenyl chloride are introduced into a solution of 2 g of 2,4,6-trimethyl benzamidine in 16 ml of dichloromethane under an inert atmosphere at about -20° C., followed by the slow addition of 2 g of NaOH dissolved in 3.2 ml of water at about -10° C. After I hour at about -5° C., the precipitate formed is isolated and the organic phase is separated and washed with 6 ml of water. After being dried over K2CO3, it is concentrated under reduced pressure to give 2.8 g of the desired product in the form of an oil, which may be used without purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05470855 |
| Quelldatensatz | uspto-grants-1995_11 |
| ORD ID | ord-80152b1af913426387206ec895462f2e |
| Quellennotiz | uspto-grants-1995_11 |