関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hippuric Acid | HCID 464 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 反応物 | 1-(4-Chlorobenzyl)pyrrolidin-3-amine dihydrochloride | HCID 18426180 | — |
| 反応物 | Dimethylaminopropyl carbodiimide hydrochloride | HCID 21899179 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 3-(N-benzoylglycyl)amino-1-(4-chlorobenzyl)pyrrolidine | HCID 9842404 | — |
反応手順
N-Benzoylglycine (9.9 mg, 0.055 mmol), 3-ethyl-1-(3-(dimethylaminopropyl)carbodiimide hydrochloride (EDCI) (10.5 mg) and 1-hydroxybenzotriazole hydrate (HOBt) (7.4 mg) were added to a solution of 3-amino-1-(4-chlorobenzyl)pyrrolidine dihydrochloride (14.2 mg, 0.050 mmol) and Et3N (15.2 mg) in CHCl3 (2.5 mL). The reaction mixture was stirred at 25° C. for 16 h, washed with 2 N aqueous NaOH (2 mL×2) and brine (1 mL). After filtration through a PTFE membrane filter, the solvent was removed under reduced pressure to afford 3-(N-benzoylglycyl)amino-1-(4-chlorobenzyl)pyrrolidine (compound No. 1) as a pale yellow oil (17.7 mg, 95%): The purity was determined by RPLC/MS (95%); ESI/MS m/e 372.0 (M++H, C20H22ClN3O2).
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-dcc9b4670f1e4ec1a467bc1e330e69da |
|---|
| 出典メモ | uspto-grants-2002_09 |
|---|
