Morpholine → 4-(4-Bromo-2-fluorobenzyl)morpholine
反応式
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6]Br)=[C:4]([F:10])[CH:3]=1.[NH:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1>CN(C)C=O>[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)=[C:4]([F:10])[CH:3]=1参加物
4
実験手順
4-Bromo-2-fluorobenzyl bromide (3.0 g) and morpholine (2.15 ml) were stirred in dimethylformamide (30 ml) at ambient temperature for 18 h. The mixture was partitioned between diethyl ether (80 ml) and water (80 ml). The aqueous phase was extracted further with diethyl ether (80 ml) and the combined organic phases were dried (magnesium sulfate) and concentrated in vacuo. The residue was purified by column chromatography, eluting with a gradient of 0-30% ethyl acetate/iso-hexane to give the product as a colourless oil (2.92 g).
後処理
- customThe mixture was partitioned between diethyl ether (80 ml) and water (80 ml)
- extractionThe aqueous phase was extracted further with diethyl ether (80 ml)
- dry with materialthe combined organic phases were dried (magnesium sulfate)
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography
- washeluting with a gradient of 0-30% ethyl acetate/iso-hexane
出典と根拠
- ORDレコード
- ord-fc119b72487d40b4896374ba98a3b5fb
- 出典データセット
- uspto-grants-2011_06
- 特許番号
- US07956084B2
反応ノート
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