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Hydrochloric Acid → 1-(4-Chlorobenzyl)-3-[(glycylamino)methyl]pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-[{N-(tert-butoxycarbonyl)glycyl)aminomethyl]-1-(4-chlorobenzyl)pyrrolidine | HCID 18426255 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-(4-Chlorobenzyl)-3-[(glycylamino)methyl]pyrrolidine | HCID 18426257 | 100.7% |
反応手順
To a solution of 3-[{N-(tert-butoxycarbonyl)glycyl}aminomethyl]-1-(4-chlorobenzyl)pyrrolidine (804 mg, 2.11 mmol) in methanol (10 mL) was added 4 N HCl in dioxane (5 mL). The solution was stirred at room temperature for 3.5 h. The reaction mixture was concentrated and 1 N NaOH solution (20 mL) was added. The mixture was extracted with dichloromethane (20 mL×3), and the combined extracts were dried over sodium sulfate and concentrated to give desired 1-(4-chlorobenzyl)-3-{(glycylamino)methyl)pyrrolidine (599 mg, 100%): The purity was determined by RPLC/MS (100%); ESI/MS m/e 282.2 (M++H, C14H20ClN3O).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06362177B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-2f47070e234a4decb121ca186beac323 |
| 出典メモ | uspto-grants-2002_03 |