HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 2-hexanesulfonyl-7-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 2-hexylthio-7-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 14100769 | — |
| Product | 2-hexanesulfonyl-7-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 14100770 | 45% |
Reaction Steps
A mixture of 6.1 g of 2-hexylthio-7-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one, 9.1 g of a 30% hydrogen peroxide solution and 14 ml of acetic acid was heated to 65°-75° C. and stirred for 2 hours and 15 minutes. After cooling, water was added to the mixture and the resulting mixture was extracted with chloroform. The organic layer was washed with a sodium thiosulfate and water respectively, and dried over anhydrous sodium sulfate anhydrate. The solvent was distilled off. The residue was recrystallized from ethanol and thus 3.2 g of 2-hexanesulfonyl-7-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. m.p. 111°-115° C. Yield 45%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04742063 |
| Source dataset | uspto-grants-1988_05 |
| ORD ID | ord-3a3efd2b85fc44b6ab0d6d5bdc9572e7 |
| Source note | uspto-grants-1988_05 |