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Methanol → Ammonium Hydroxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 2-(Trifluoromethyl)imidazo[1,2-a]pyrazine | HCID 3231306 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 生成物 | Ammonium Hydroxide | HCID 14923 | 1% |
| 生成物 | 2-(trifluoromethyl)-5H,6H,7H,8H-imidazo[1,2-a]pyrazine | HCID 14719928 | — |
反応手順
To a solution of 2-(trifluoromethyl)imidazo[1,2-a]pyrazine (2.0 g, 10.46 mmol, from Step A) in methanol (100 mL) was added 10% palladium on carbon (400 mg). The mixture was stirred under atmospheric hydrogen at ambient temperature for 14 h. The mixture was filtered through Celite and washed three times with methanol. The filtrate was concentrated and purified by flash chromatography (silica gel, 10% methanol in ethyl acetate, then 15% methanol in chloroform with 1% aqueous ammonium hydroxide) to give the title compound as a solid. 1H NMR (500 MHz, CDCl3): δ 1.93 (bs, 1H), 3.26 (t, 2H, J=5.5 Hz), 3.99 (t, 2H, J=5.5 Hz), 4.10 (s, 1H), 7.16 (s, 1H). ESI-MS 192 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07482336B2 |
| 出典データセット | uspto-grants-2009_01 |
| ORD ID | ord-5042aaefcc7d45d2ad98a833fcc93fa3 |
| 出典メモ | uspto-grants-2009_01 |