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Water → N-[4-[3-(1-adamantyl)-4-methoxy benzamido]-benzoyl]pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-(Pyrrolidin-1-ylcarbonyl)aniline | HCID 577800 | — |
| 反応物 | 3-(1-Adamantyl)-4-methoxybenzoyl chloride | HCID 10804497 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[4-[3-(1-adamantyl)-4-methoxy benzamido]-benzoyl]pyrrolidine | HCID 19762696 | 73% |
反応手順
1.7 g (9 mmoles) of N-p-aminobenzoyl pyrrolidine and 1 g (10 mmoles) of triethylamine are dissolved in 30 ml of dichloromethane. With stirring, 2.8 g (9 mmoles) of 3-(1-adamantyl)-4-methoxybenzoyl chloride dissolved in 60 ml of dichloromethane are added. The reaction mixture is stirred for 16 hours, at which point water is added and the reaction mixture is extracted with dichloromethane. The extract is washed with water, extracted with methylene chloride and dried on MgSO4. The solvents are evaporated and the residue (yellow foam) is crystallized in ethyl acetate to give 3.0 g (73% yield) of N-[4-[3-(1-adamantyl)-4-methoxy benzamido]-benzoyl] pyrrolidine which melts at 239°-242° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05212203 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-c48105e083704c33a04f4f9408d6ac74 |
| 出典メモ | uspto-grants-1993_05 |