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3-Acetamidophthalic Anhydride → alpha-Hexyl-4-{[3-(acetylamino)-2-carboxybenzoyl]-amino}-1H-imidazole-1-acetic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Acetamidophthalic Anhydride | HCID 226121 | — |
| 反応物 | Ethyl 2-(4-nitro-1H-imidazole-1-yl)octanoate | HCID 10062368 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | alpha-Hexyl-4-{[3-(acetylamino)-2-carboxybenzoyl]-amino}-1H-imidazole-1-acetic acid ethyl ester | HCID 54002110 | 21.7% |
反応手順
Following the procedure of Example 2, 1.54 g of 4-nitro-α-hexyl-1H-imidazole-1-acetic acid ethyl ester were hydrogenated to the corresponding amine and allowed to react with 1.12 g of 3-acetamidophthalic anhydride in ethyl acetate. After stirring at room temperature, the solution was concentrated in vacuo and a small amount ethyl acetate added. After sitting overnight, the resulting solid was collected by filtration. Crystallization from hot ethyl acetate/methanol/ hexanes provided 0.54 g of the desired intermediate, m.p. 144'-145° C. NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05563278 |
| 出典データセット | uspto-grants-1996_10 |
| ORD ID | ord-bd31e7c3ee5347f9bb3c6391c432df1a |
| 出典メモ | uspto-grants-1996_10 |