関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Urea | HCID 1176 | — |
| 反応物 | Methyl Isocyanate | HCID 12228 | — |
| 反応物 | 3-(Trichloromethyl)-1,2,4-thiadiazol-5-amine | HCID 602848 | — |
| 生成物 | 1,3-Dimethyl-5-(3-Trichloromethyl-1,2,4-thiadiazol-5-yl)biuret | HCID 23341244 | 65% |
反応手順
A glass pressure vessel was charged with 27.5 grams (0.13 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole, 17.9 grams (0.31 mole) methyl isocyanate, and 250 milliliters benzene. A magnetic stirring bar was added and the vessel sealed. The stirred reaction mixture was heated at 145° C. for 1.5 hours and then allowed to cool to room temperature where a urea by-product precipitates. The by-product was removed by filtration and the filtrate concentrated in vacuo to leave 27.2 grams (65% yield) of product. Recrystallization from methanol gave an analytically pure sample; m.p. 94° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04224449 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-f015a097b8da43e99cb995089103c23a |
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| 出典メモ | uspto-grants-1980_09 |
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