関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitroethane | HCID 6587 | — |
| 反応物 | Phenyl isocyanate | HCID 7672 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | tert-Butyl (6-ethynyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylcarbamate | HCID 57691050 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Tert-butyl (6-(3-methylisoxazol-5-yl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylcarbamate | HCID 57691036 | — |
反応手順
To a solution of nitroethane (1.02 ml, 14.3 mmol) in benzene (50 mL) was added phenyl isocyanate (3.12 ml, 28.5 mmol). The mixture was stirred at 50° C. for twenty minutes followed by the addition of tert-butyl (6-ethynyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylcarbamate (3.00 g, 11.0 mmol) and triethylamine (0.0765 ml, 0.549 mmol). The mixture was stirred at 50° C. for six hours then at room temperature overnight. The mixture was cooled to room temperature, filtered and the resulting brown precipitate was washed with additional benzene. The filtrate was concentrated to yield the product as a black solid. MS m/z=331.1 [M+1]+. Calc'd for C15H18N6O3: 330.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524900B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-d952825d729b4d20be4a45b727aa6332 |
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| 出典メモ | uspto-grants-2013_09 |
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