Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
O-Xylene → 2-benzylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | O-Xylene | HCID 7237 | — |
| 반응물 | 1,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)- | HCID 99285 | — |
| 반응물 | Ethyl 3-ethoxy-2-propenoate | HCID 221780 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-benzylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 14254429 | 54% |
반응 단계
Fifteen point five (15.5) grams of 2-amino-5-benzylthio-1,3,4-thiadiazole, 10 g of ethyl 3-ethoxypropenoate, 15 g of polyphosphoric acid and 15 ml of xylene were mixed and vigorously stirred for 30 minutes. After the reaction was finished, the reaction mixture was cooled. Water was added to the reaction mixture and the mixture was extracted with toluene. 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, the residue was recrystallized from an ethanol/hexane mixture, and thus 10.3 g of 2-benzylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. Yield 54%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04985432 |
| 출처 데이터셋 | uspto-grants-1991_01 |
| ORD ID | ord-782d3eda1be948168e68848e8081f808 |
| 출처 메모 | uspto-grants-1991_01 |