Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)- → 2-benzylthio-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)- | HCID 99285 | — |
| 반응물 | Ethyl 3-hydroxy-2-methylprop-2-enoate | HCID 521546 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-benzylthio-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 14254420 | 61% |
반응 단계
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%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04985432 |
| 출처 데이터셋 | uspto-grants-1991_01 |
| ORD ID | ord-35ae8714201243f5b91fb10764566b0e |
| 출처 메모 | uspto-grants-1991_01 |