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2,6-Difluorobenzoyl chloride → 2-(3,4,5-Trimethoxyphenylamino)-6-[4-(2,6-difluorophenylcarbonyl)-amino phenyl]-pyrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Difluorobenzoyl chloride | HCID 87438 | — |
| 反応物 | 2-(3,4,5-Trimethoxyphenylamino)-6-(4-aminophenyloxy)-pyrazine | HCID 59343439 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(3,4,5-Trimethoxyphenylamino)-6-[4-(2,6-difluorophenylcarbonyl)-amino phenyl]-pyrazine | HCID 66912566 | 30% |
反応手順
Using Method LL with 2-(3,4,5-trimethoxyphenylamino)-6-(4-aminophenyloxy)-pyrazine (50 mg, 0.14 mmol) and 2,6-difluoro-phenylcarbonyl chloride (30 mg, 0.17 mmol), and purification by column chromatography (AcOEt), the title compound was obtained (21 mg). Yield: 30%. 1H NMR (250 MHz, DMSO-d6) δ 3.65 (s, 3H, [CH3O]4), 3.85 (s, 6H, [CH3O]3+5), 7.27 (s, 2H, Harom2′+6′), 7.45-7.47 (m, 1H, Harom 3″), 7.79-7.84 (m, 2H, Harom 4″+5″), 7.86 (d, 2H, Harom 3+5, J=8.3 Hz), 8.14 (s, 1H, HPz 5), 8.15 (d, 2H, Harom 2+6, J=6.7 Hz), 8.52 (s, 1H, HPz 3), 9.56 (s, 1H, NH), 10.61 (s, 1H, NHamide). m/z 493.2 [(M+H)+ calcd for C26H22F2N4O6 492.2].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737152B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-41b43b43a566470582a78c52bf67495b |
| 出典メモ | uspto-grants-2010_06 |