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benzyl (3-(2-(dimethylamino)ethoxy)-1-methyl-1H-pyrazol-5-yl)carbamate → 3-[2-(dimethylamino)ethoxy]-1-methyl-1H-pyrazol-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | benzyl (3-(2-(dimethylamino)ethoxy)-1-methyl-1H-pyrazol-5-yl)carbamate | HCID 86679669 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-[2-(dimethylamino)ethoxy]-1-methyl-1H-pyrazol-5-amine | HCID 86679670 | 79.1% |
反応手順
A mixture of benzyl (3-(2-(dimethylamino)ethoxy)-1-methyl-1H-pyrazol-5-yl)carbamate (1.42 g, 4.46 mmol) and 10% Pd/C (0.2 g) in MeOH (40 mL) was hydrogenated with fully inflated H2 balloon at rt overnight. The mixture was filtered and the filtrate was concentrated in vacuo to give the title compound (0.65 g, 79% yield) as a pale solid. 1H NMR (400 MHz, CDCl3) δ ppm 5.04 (s, 1H), 4.19-4.16 (t, 2H), 3.51 (s, 3H), 3.45 (bs, 2H), 2.67-2.64 (t, 2H), 2.32 (s, 6H). m/z for C8H16N4O 185.14 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09040547B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-e6062623629c4ccbb420a70d63da79f3 |
| 出典メモ | uspto-grants-2015_05 |