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Hydrochloric Acid → Methyl 1-(4-methoxybenzyl)-5-oxopyrrolidine-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Dimethyl itaconate | HCID 69240 | — |
| 反応物 | 4-Methoxybenzylamine | HCID 75452 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 1-(4-methoxybenzyl)-5-oxopyrrolidine-3-carboxylate | HCID 4093874 | — |
反応手順
To 4-metoxybenzylamine (42 g, 0.306 mol) in methanol (40 mL) at 0° C. was added the dimethyl itaconate (48 g, 0.306 mol) in methanol (13 mL). The solution was stirred at room temperature for 4 days. 1N HCl was added to the solution followed by ether. The two layers were separated and the aqueous phase extracted with ether. The combined organic phases were dried (MgSO4). Upon filtration of the drying agent the desired material 79 precipitated from solution that was collected and dried under vacuum. 23.26 g, 29%. MS, m/z (relative intensity): 264 [M+H, 100%]. Anal. Calcd for C14H17N1O4: C, 63.87; H, 6.51; N, 5.32. Found: C, 63.96; H, 6.55; N, 5.29.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07189747B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-d3d90baa136e4172aba3ef183fdb5188 |
| 出典メモ | uspto-grants-2007_03 |