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Dimethylamine → 2-(N,N-Dimethylamino)-6-Iodopyrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | 2,6-Diiodopyrazine | HCID 11002078 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(N,N-Dimethylamino)-6-Iodopyrazine | HCID 15750131 | — |
反応手順
A solution of 2,6-diiodopyrazine (6 g, 18.1 mmol) in methanol (50 ml) and dimethylamine (40% aqueous solution, 200 ml) was heated at reflux for 1 h. The methanol was removed under vacuum, the aqueous saturated with potassium carbonate and extracted with dichloromethane (3×100 ml). The combined extracts were dried (Na2SO4), evaporated and the residue purified by chromatography through silica-gel eluting with dichloromethane. The product (4 g) was obtained as a low melting solid, m.p. 46°-48° C., m/e 249 (M+); δ (360 MHz, CDCl3) 3.10 (6H, s, 2×Me); 7.87 (1H, s, pyrazine-H); 8.01 (1H, s, pyrazine-H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05260293 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-5e6592da0d65436e8bf54cdc85ddec51 |
| 出典メモ | uspto-grants-1993_11 |