化工社化工社 化学情報印刷レポート · 研究参考用
1,4-Dibromobutane → 1-acetyl-N-benzylcyclopentane carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,4-Dibromobutane | HCID 8056 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Acetoacetobenzylamide | HCID 70159 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-acetyl-N-benzylcyclopentane carboxamide | HCID 118390123 | 54.2% |
反応手順
To a solution of N-benzyl-3-oxobutanamide (100.00 g, 522.93 mmol), K2CO3 (216.50 g, 1568.79 mmol) in DMF (1 L) was added 1,4-dibromobutane (169.36 g, 784.4 mmol) dropwise at rt. After addition, the reaction mixture was stirred at rt overnight and concentrated in vacuo. The residue was added water (500 mL) and extracted with EtOAc (500 mL×3). The combined organic phases were washed with brine (500 mL×3), dried over anhydrous Na2SO4, then filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/PE (v/v)=1/8) to give the product as a white solid (69.50 g, 54%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09403801B2 |
| 出典データセット | uspto-grants-2016_08 |
| ORD ID | ord-71f4774d367f43dabb4a5bfde6710acd |
| 出典メモ | uspto-grants-2016_08 |