HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Chlorobenzene → 2-heptylthio-7-hydroxy-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Chlorobenzene | HCID 7964 | — |
| Edukt | 1,3,4-Thiadiazole, 2-amino-5-(heptylthio)- | HCID 534458 | — |
| Edukt | Bis(2,4,6-trichlorophenyl) methylpropanedioate | HCID 12320374 | — |
| Lösungsmittel | Hexane | HCID 8058 | — |
| Produkt | 2-heptylthio-7-hydroxy-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 136120198 | 78% |
Reaktionsschritte
A mixture of 19.7 g of the thus obtained 2-amino-5-heptylthio-1,3,4-thiadiazole, 40.9 g of bis(2,4,6-trichlorophenyl)-2-methyl-malonate and 55 ml of chlorobenzene was stirred at 140°~144° C. for 45 minutes. After cooling, n-hexane was added thereto, the precipitate was collected by filtration. Further n-hexane was added to the filtrate, and the precipitate was collected The collected precipitates were combined. The combined precipitate was washed with n-hexane and thus 21.2 g of 2-heptylthio-7-hydroxy-6-methyl-5H-1,3,4-thiadiazolo-[3,2-a] pyrimidin-5-one was obtained. m.p. 141°~143° C. Yield 78%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04971971 |
| Quelldatensatz | uspto-grants-1990_11 |
| ORD ID | ord-d294e1d6a6af4952ac6b990fe50a2482 |
| Quellennotiz | uspto-grants-1990_11 |