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Formic Acid → 4-(2-methyl-1H-imidazol-1-yl)aniline
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 | 2-Methyl-1-(4-nitrophenyl)-1H-imidazole | HCID 10013118 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(2-methyl-1H-imidazol-1-yl)aniline | HCID 3157478 | 75.8% |
反応手順
A mixture of 54.0 g of 2-methyl-1-(p-nitrophenyl)imidazole, 2.87 g of palladium black, 36.7 g of sodium formate and 47.4 ml of formic acid in 1100 ml of methyl alcohol is stirred at room temperature for 18 hours under a hydrogen atmosphere. The mixture is filtered and the filtrate evaporated to a residue. The residue is partitioned between saturated potassium bicarbonate and chloroform. The organic layer is dried and passed through a pad of hydrous magnesium silicate. The filtrate is evaporated to a residue which is crystallized from ether:ethanol to give 34.9 g of the desired product as a solid, m.p. 108°-110° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05225425 |
| 出典データセット | uspto-grants-1993_07 |
| ORD ID | ord-62bbf20c3e1e4af38a3f7fff08dd1660 |
| 出典メモ | uspto-grants-1993_07 |