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Benzil → 3-(4,5-diphenyl-1H-imidazol-2-yl)propionic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzil | HCID 8651 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Methyl 4,4-dimethoxybutanoate | HCID 350846 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(4,5-diphenyl-1H-imidazol-2-yl)propionic acid methyl ester | HCID 68413807 | — |
反応手順
A solution of 1 g of benzil, 1.01 g of methyl 4,4-dimethoxybutyrate and 2.87 g of ammonium acetate in 23 mL of acetic acid was refluxed for 5 h. The mixture was poured into water, basified with a 25% aq. ammonium hydroxide solution and extracted with DCM. The organic phase was dried over anh. Na2SO4 and concentrated in vacuo. The resulting crude material was purified by CC using heptane/EtOAc from 85/15 to 0/100 as eluant to yield 633 mg of 3-(4,5-diphenyl-1H-imidazol-2-yl)-propionic acid methyl ester as a yellowish solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202885B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-892bcec21f6c40609c2057332dd0077b |
| 出典メモ | uspto-grants-2012_06 |