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Morpholine → 4-(2-Fluoro-4-nitrophenyl)morpholine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(2-Fluoro-4-nitrophenyl)morpholine | HCID 2905489 | 99% |
反応手順
To a solution of morpholine (12.04 g, 0.14 mol) and Et3N (13.97 g, 0.14 mol) in EtOAc was added 3,4-difluoronitrobenzene (20.0 g, 0.13 mol) dropwise in an ice bath. The reaction mixture was warmed to rt slowly, stirred at rt overnight, and then filtered. The filter cake was washed with water, dried in vacuo to obtain the 1st crop of product. The organic phase was separated from the filtrate, and the water phase was washed with EtOAc. The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo to obtain the 2nd crop of product. The solids of 1st crop and 2nd crop were combined to give the title compound as a yellow solid (28.0 g, 99%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434695B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-50124155b9af4ad6bdae3bd136f7e5aa |
| 出典メモ | uspto-grants-2016_09 |