Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloroform → 2-benzylthio-6-methoxy-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloroform | HCID 6212 | — |
| 반응물 | 1,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)- | HCID 99285 | — |
| 반응물 | Propyl 3-hydroxy-2-methoxyprop-2-enoate | HCID 71336589 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-benzylthio-6-methoxy-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 14254423 | 93% |
반응 단계
Four (4) grams of the thus obtained 2-amino-5-benzylthio-1,3,4-thiadiazole, 3.2 g of propyl 3-hydroxy-2-methoxy-propenoate and 11 g of polyphosphoric acid were heated to 135° C. and stirred for 20 minutes. After cooling, chloroform and water were added thereto, extraction was carried out. The organic layer was washed with an aqueous sodium hydrogen carbonate solution and water, and dried over anhydrous sodium sulfate. The solvent was distilled off and the residue was washed with an ethanol/hexane mixture and 5.1 g of 2-benzylthio-6-methoxy-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. Yield 93%. The compound was recrystallized from ethanol. m.p. 145°-147° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04985432 |
| 출처 데이터셋 | uspto-grants-1991_01 |
| ORD ID | ord-ca8a64f9a8e3465db27d2aec6e5c920f |
| 출처 메모 | uspto-grants-1991_01 |