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O-Xylene → 2-benzylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-Xylene | HCID 7237 | — |
| 反応物 | 1,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)- | HCID 99285 | — |
| 反応物 | Ethyl 3-ethoxy-2-propenoate | HCID 221780 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-benzylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 14254429 | 54% |
反応手順
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%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04985432 |
| 出典データセット | uspto-grants-1991_01 |
| ORD ID | ord-782d3eda1be948168e68848e8081f808 |
| 出典メモ | uspto-grants-1991_01 |