HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)- → 2-benzylthio-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)- | HCID 99285 | — |
| Edukt | Ethyl 3-hydroxy-2-methylprop-2-enoate | HCID 521546 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 2-benzylthio-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 14254420 | 61% |
Reaktionsschritte
Five point six (5.6) grams of the thus obtained 2-amino-5-benzylthio-1,3,4-thiadiazole and 3.6 g of ethyl 3-hydroxy-2-methyl-2-propenoate were mixed with 7.5 g of polyphosphoric acid, and the mixture was stirred at 130°-150° C. for 45 minutes. After cooling, water was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed with an aqueous sodium hydrogen carbonate solution and water respectively, and dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was recrystallized from ethanol. Thus 4.4 g of 2-benzylthio-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. m.p. 130°-132° C. Yield 61%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04985432 |
| Quelldatensatz | uspto-grants-1991_01 |
| ORD ID | ord-35ae8714201243f5b91fb10764566b0e |
| Quellennotiz | uspto-grants-1991_01 |