関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrazinecarboxaldehyde | HCID 12229 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | Methyl 5-bromo-3-cyanopyridin-2-ylcarbamate | HCID 86705383 | — |
| 生成物 | 9-bromopyrido[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5(6H)-one | HCID 136338032 | 60% |
反応手順
Formyl hydrazine (60 mg, 1.0 mmol) was added to a solution of methyl 5-bromo-3-cyanopyridin-2-ylcarbamate (255 mg, 1.0 mmol) in 1-methylpyrrolidinone (5 mL). The resulting mixture was stirred at 120° C. for 3 h. The mixture was cooled to room temperature and poured into ice-water (20 mL). The resulting solid was separated by filtration, washed with water and hexanes and dried under vacuum to afford the title compound (160 mg, 60%). 1H NMR (400 MHz, DMSO-d6) δ 8.60 (s, 1H), 8.70 (s, 1H), 8.80 (s, 1H), 13.00 (br s, 1H). [M+H]=266.3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09284335B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-b655ac79572347d6adb6b7d29dc6112e |
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| 出典メモ | uspto-grants-2016_03 |
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