関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Morpholinobenzonitrile | HCID 394808 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Morpholinobenzylamine | HCID 2776458 | 58.9% |
反応手順
Into a 50-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 4-morpholinobenzonitrile (200 mg, 1.06 mmol, 1.00 equiv) in tetrahydrofuran (10 mL), and LiAlH4 (400 mg, 10.53 mmol, 10.00 equiv). The resulting solution was stirred for 3 h at 60° C. The reaction was then quenched with 1 N NaOH. The solids were removed by filtration. The resulting solution was extracted with 3×20 mL of dichloromethane and the organic layers combined, dried over NaSO4, and concentrated under vacuum. The product was obtained as 120 mg (58%) of a yellow solid. 1H-NMR (300 MHz, CDCl3, ppm): δ 7.26 (m, 2H). 6.91 (m, 2H), 3.87 (m, 6H), 3.16 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09301951B2 |
|---|
| 出典データセット | uspto-grants-2016_04 |
|---|
| ORD ID | ord-4b70c88b4d004e3dafca5e9b198eb315 |
|---|
| 出典メモ | uspto-grants-2016_04 |
|---|