関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Bromoaniline | HCID 11562 | — |
| 反応物 | Bis(2-bromoethyl) ether | HCID 21521 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(3-Bromophenyl)morpholine | HCID 4961268 | 43% |
反応手順
3-Bromoaniline (3.0 mL, 4.7 g, 28 mmol), 2-bromoethylether (4.2 mL, 7.7 g, 33 mmol) and diisopropylethylamine (15 mL, 11 g, 86 mmol) were dissolved in anhydrous DMF (20 mL) under inert gas atmosphere and heated to 100° C. for 6 h. After cooling to room temperature the mixture was poured into water (300 mL) and extracted with EtOAc. The combined organic layers were washed with brine, dried Na2SO4), filtered and evaporated to dryness. Purification of the residue by flash chromatography afforded 2.9 g (12 mmol, 43% yield) of 4-(3-bromophenyl)morpholine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06608052B2 |
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| 出典データセット | uspto-grants-2003_08 |
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| ORD ID | ord-1c187fb966aa4e42b729832344ceba1e |
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| 出典メモ | uspto-grants-2003_08 |
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