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Triethylamine → (R)-1-(4-chlorobenzyl)-3-[[N-(4-dimethylaminobenzoyl)glycyl]amino]pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-(Dimethylamino)benzoic acid | HCID 12092 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | (R)-1-(4-chlorobenzyl)-3-(glycylamino)pyrrolidine | HCID 54551710 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | (R)-1-(4-chlorobenzyl)-3-[[N-(4-dimethylaminobenzoyl)glycyl]amino]pyrrolidine | HCID 69215736 | — |
反応手順
A solution of (R)-1-(4-chlorobenzyl)-3-(glycylamino)pyrrolidine (13.8 mg, 0.052 mmol) in CHCl3 (2 mL) was treated with Et3N (0.021 mL, 0.15 mmol), 4-(dimethylamino)benzoic acid (10 mg, 0.061 mmol), EDCI (10.2 mg, 0.053 mmol) and HOBt (7.5 mg, 0.055 mmol). The reaction mixture was stirred at room temperature for 16 h. The solution was washed with 2 N aqueous NaOH solution (2 mL×2) and brine (2 mL), and dried by filtration through a PTFE membrane using CH2Cl2 (3 mL). Concentration afforded the desired material (compound No. 952) (24.9 mg, quant): The purity was determined by RPLC/MS (91%); ESI/MS m/e 415.0 (M++H, C22H27ClN4O2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06451842B1 |
| 出典データセット | uspto-grants-2002_09 |
| ORD ID | ord-c1216aed88664c66a1c17263040677a0 |
| 出典メモ | uspto-grants-2002_09 |