関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 4-Benzylmorpholine-2-carboxylic acid hydrochloride | HCID 2776352 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 4-benzyl-N,N-dimethylmorpholine-2-carboxamide | HCID 71138511 | 83.4% |
反応手順
Oxalyl chloride (372 μL, 4.27 mmol) was added to a mixture of 4-benzylmorpholine-2-carboxilic acid hydrochloride (1.00 g, 3.88 mmol) and N,N-dimethylformamide (15.0 μL, 0.194 mmol) in DCE (20 mL). The mixture was heated at 65° C. for 3 hours. After cooling to 0° C., Me2NH (2M solution in THF, 9.70 mL, 19.4 mmol) was added. The mixture was stirred at room temperature for 4 hours. The mixture was concentrated and the residue was diluted with water and extracted with EtOAc (3×). The combined organic layers were dried over anhydrous Na2SO4 and concentrated to afford desired product (803 mg, 83.4%) as brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08962619B2 |
|---|
| 出典データセット | uspto-grants-2015_02 |
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| ORD ID | ord-c1678fe17f3b4520b0d5f80b86a22c23 |
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| 出典メモ | uspto-grants-2015_02 |
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