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Formic Acid → 3-(4-Methyl-1H-imidazol-1-yl)benzenamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Sodium Formate | HCID 2723810 | — |
| 反応物 | 4-methyl-1-(3-nitrophenyl)-1H-imidazole | HCID 15030166 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(4-Methyl-1H-imidazol-1-yl)benzenamine | HCID 15030167 | 82.8% |
反応手順
A mixture of 14.6 g of 4-methyl-1-(3-nitrophenyl)-1H-imidazole, 766 mg of palladium black, 19.6 g of sodium formate, 12.8 ml of formic acid in 300 ml of methyl alcohol is stirred for 18 hours under a hydrogen atmosphere. The mixture is filtered through diatomaceous earth and the filtrate evaporated to a residue. The residue is partitioned between saturate potassium bicarbonate and chloroform. The organic layer is dried and evaporated to a residue which is dissolved in a minimum of chloroform and passed through a pad of hydrous magnesium silicate. The filtrate is evaporated to a residue which is stirred with ether and the resulting solid filtered and air dried to give 10.3 g of the desired product as a solid, m.p. 117°-119° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05077409 |
| 出典データセット | uspto-grants-1991_12 |
| ORD ID | ord-dbd2f11aee69470a843d0f38a84286c7 |
| 出典メモ | uspto-grants-1991_12 |