化工社化工社 化学情報印刷レポート · 研究参考用
1-Methylpiperazin-2-one → Methyl 2-(4-methyl-3-oxopiperazin-1-yl)pyrimidine-5-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Methylpiperazin-2-one | HCID 4399042 | — |
| 反応物 | Methyl 2-chloropyrimidine-5-carboxylate | HCID 12627752 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 2-(4-methyl-3-oxopiperazin-1-yl)pyrimidine-5-carboxylate | HCID 66589656 | 57% |
反応手順
A solution of 1-methylpiperazin-2-one (198 mg, 1.74 mmol) in dichloromethane (4.00 mL) was added to a stirred solution of methyl 2-chloropyrimidine-5-carboxylate (300 mg, 1.74 mmol) in dichloromethane (4.70 mL) at 25° C. The resulting solution was stirred at room temperature for 4 h under nitrogen. The reaction mixture was concentrated and dissolved in ethyl acetate (25 ml) and NaOH (50 ml, 1M aqueous solution). The organic layer was washed with ethyl acetate (25 ml). The organic layers were combined and washed with brine (50 ml), dried using MgSO4, filtered and evaporated to dryness to afford methyl 2-(4-methyl-3-oxopiperazin-1-yl)pyrimidine-5-carboxylate (246 mg, 57%) as a cream solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737149B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-864fcefcabf84f04b65128176e6490f0 |
| 出典メモ | uspto-grants-2010_06 |