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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 69995760、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | Cyclopropylamine | HCID 69828 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 1-benzyl hydrogen (R)-pyrrolidine-1,2-dicarboxylate | HCID 111208 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | HCID 69995760 | HCID 69995760 | 92.5% |
反応手順
To a mixture of (+)-carbobenzyloxy-D-proline (1.5 g, 6 mmol), EDAC (2.3 g, 2 eq.), HOBt (0.8 g, 2 eq.) in DMF (20 mL) was added triethylamine (1.5 mL) and cyclopropylamine (0.8 mL, 2 eq.). After stirring at RT for 18 h, the reaction was basified with sodium bicarbonate, poured to brine, and followed by extraction with dichloromethane. After concentration of the combined extracts, the residue was purified on a silica gel column eluting with 100% EtOAc to give 1.6 g (92%) of (R)-2-cyclopropylcarbamoyl-pyrrolidine-1-carboxylic acid benzyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06599902B2 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-763ffc04425e4213bbe1c3d5288b54ec |
| 出典メモ | uspto-grants-2003_07 |