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Phosgene → 1,3,4-Thiadiazole, 2-isocyanato-5-(trifluoromethyl)-, dimer
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | 1,3,4-Thiadiazol-2-amine, 5-(trifluoromethyl)- | HCID 82634 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1,3,4-Thiadiazole, 2-isocyanato-5-(trifluoromethyl)-, dimer | HCID 76871835 | — |
反応手順
A saturated solution of phosgene in ethyl acetate (100 ml) was charged into a glass reaction vessel equipped with a mechanical stirrer. A slurry of 5-trifluoromethyl-2-amino-1,3,4-thiadiazole (45 grams) in ethyl acetate (300 ml) was added to the reaction vessel and the resulting mixture was stirred for a period of about 16 hours resulting in the formation of a precipitate. The reaction mixture was then purged with nitrogen gas to remove unreacted phosgene. The purged mixture was filtered to recover 48 grams of a white solid. This solid was recrystallized from dimethyl formamide to yield the desired product 5-trifluoromethyl-1,3,4-thiadiazol-2-yl isocyanate dimer.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03944409 |
| 出典データセット | uspto-grants-1976_03 |
| ORD ID | ord-a64b8339e7684b25b9ef7888cb17d917 |
| 出典メモ | uspto-grants-1976_03 |