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Ethyl Acetate → 4-(4-Biphenylylmethoxy)phenyl-N-[2-(N,N-dimethylamino)ethyl]acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1H-1,2,4-Triazole | HCID 9257 | — |
| 反応物 | N,N-Dimethylethylenediamine | HCID 66053 | — |
| 反応物 | Methyl 4-(4-biphenylylmethoxy)phenylacetate | HCID 18508368 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-(4-Biphenylylmethoxy)phenyl-N-[2-(N,N-dimethylamino)ethyl]acetamide | HCID 9910268 | 102.2% |
反応手順
A solution of methyl 4-(4-biphenylylmethoxy)phenylacetate (60.0 g), N,N-dimethylethylenediamine (47.7 g), and 1H-1,2,4-triazole (12.6 g) in toluene (120 ml) was stirred under nitrogen at 100° C. for 8 hr and cooled until the temperature of the reaction mixture was reached to 60±2° C., to which ethyl acetate (240 ml) was added for 20 min. The reaction mixture was further heated under reflux for additional 30 min, left to stand at room temperature over night and stirred in an ice bath for 2 hr. The precipitate was collected by filtration and washed with ethyl acetate (120 ml) to obtain the titled compound (71.7 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06586475B1 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-308277ab1f71480a8c53ba4126813c84 |
| 出典メモ | uspto-grants-2003_07 |