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Chlorobenzene → 2-benzylthio-7-hydroxy-6-methyl-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 | Chlorobenzene | HCID 7964 | — |
| 反応物 | 1,3,4-Thiadiazol-2-amine, 5-((phenylmethyl)thio)- | HCID 99285 | — |
| 反応物 | Bis(2,4,6-trichlorophenyl) methylpropanedioate | HCID 12320374 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 2-benzylthio-7-hydroxy-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one | HCID 136087661 | 91% |
反応手順
A mixture of 19.3 g of 2-amino-5-benzylthio-1,3,4-thiadiazole, 41.3 g of bis(2,4,6-trichlorophenyl) 2-methylmalonate and 60 ml of chlorobenzene was stirred at 135°-140° C. for 1 hour. After cooling, n-hexane was added to the reaction mixture and the formed precipitate was separated by filtration. The separated precipitate was washed with n-hexane and thus 23.9 g of 2-benzylthio-7-hydroxy-6-methyl-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. m.p. 247°-250° C. Yield 91%.
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-5754043e082043a497ebabbfb9547b00 |
| 出典メモ | uspto-grants-1991_01 |