関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | O-Phenylenediamine | HCID 7243 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Diethyl cyanophosphonate | HCID 76257 | — |
| 反応物 | 3-Amino-6-bromopyrazine-2-carboxylic acid | HCID 18521600 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 52937760 | HCID 52937760 | 60.4% |
反応手順
A mixture of 3-amino-6-bromo-pyrazine-2-carboxylic acid (10 g, 45.87 mmol), benzene-1,2-diamine (5.45 g, 50.46 mmol), diethoxyphosphorylformonitrile (8.23 g, 50.46 mmol) and triethylamine (12.79 mL, 91.74 mmol) in DME (30 mL) was heated in the microwave at 170° C. for 40 minutes. The mixture was allowed to cool and water was added. The resultant dark-coloured precipitate was dissolved in EtOAc and stirred with charcoal for 30 minutes. After filtering through celite, the filtrate was concentrated in vacuo to give the product as a yellow solid (8.04 g, 60% Yield). 1H NMR (400 MHz, DMSO) 7.22-7.32 (2H, m), 7.55 (1H, d), 7.75 (1H, d), 7.8 (1 h, br s), 8.8 (1H, br s), 13.1 (1H, s); MS (ES+) 291
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841308B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-3098fade2ad445e28fe562e67f568c00 |
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| 出典メモ | uspto-grants-2014_09 |
|---|