参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 1,4-氧氮六环 | HCID 8083 | — |
| 反应物 | Nitrobenzoic Acid | HCID 8497 | — |
| 反应物 | 1-羟基苯并三唑(HOBT) | HCID 75771 | — |
| 反应物 | 1-乙基-(3-二甲基氨基丙基)碳酰二亚胺盐酸盐 | HCID 2723939 | — |
| 溶剂 | 三氯甲烷 | HCID 6212 | — |
| 溶剂 | 二氯甲烷 | HCID 6344 | — |
| 溶剂 | 四氢呋喃 | HCID 8028 | — |
| 产物 | Morpholino(3-nitrophenyl)methanone | HCID 225453 | 89.8% |
反应步骤
In tetrahydrofuran (100 ml) and dichloromethane (100 ml), 3-nitrobenzoic acid (7.58 g) was dissolved. Then 1-hydroxybenzotriazole (6.74 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (9.57 g), and morpholine (9.47 g) were added to the solution. The mixture was stirred at room temperature overnight. After the reaction was completed, chloroform was added to the solution. The mixture was washed with 1N-HCl aqueous solution, 1N-NaOH aqueous solution, and distilled water. The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (Kieselgel 60=160 g, ethyl acetate) to obtain the above-captioned compound ([13]-(132)-158) (9.62 g) as white crystals.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US05731310 |
|---|
| 来源数据集 | uspto-grants-1998_03 |
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| ORD ID | ord-92408f87220947e8aa462aa1b48b9d43 |
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| 来源说明 | uspto-grants-1998_03 |
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