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Hexane → Tert-butyl 4-(5-ethylpyrimidin-2-yl)piperazine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Piperazine-1-carboxylic acid | HCID 131766 | — |
| 反応物 | 2-Chloro-5-ethylpyrimidine | HCID 3572763 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Tert-butyl 4-(5-ethylpyrimidin-2-yl)piperazine-1-carboxylate | HCID 53305712 | 41% |
反応手順
To piperazine-1-carboxylic acid .tert.-butyl ester (3.543 mmol) in EtOH (13 ml), triethylamine (1.5 ml) and 2-chloro-5-ethyl-pyrimidine (3.540 mmol) are added. The mixture is refluxed with stirring for 6 h. After cooling at room temperature, the reaction mixture is quenched with an ice water and extracted with AcOEt. The organic layer is washed with brine, dried over magnesium sulfate and concentrated to give the product in 41% yield. Rf=0.45 (n-hexane:AcOEt=10:1) 1H NMR(400 MHz, CDCl3) δ 1.19 (t, 3H), 1.49 (s, 9H), 2.47 (q, 2H), 3.49 (dd, 4H), 3.76 (dd, 4H), 8.18 (s, 2H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07452886B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-89bb9428f6594941ac30e5acc50f4b5d |
| 出典メモ | uspto-grants-2008_11 |