Morpholine → 4-(5-bromopyridin-2-yl)morpholine
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5](Cl)=[N:6][CH:7]=1.[NH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1>CN(C)C(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[N:6][CH:7]=1参加物
4
反応条件
- 温度
- 130 °C
実験手順
5-Bromo-2-chloropyridine (5.0 g) was mixed with N,N-dimethylacetamide (25 ml), and morpholine (23 ml) was added thereto, followed by stirring at 130° C. for 2 days. The reaction mixture was concentrated under reduced pressure, and water was added to the residue, followed by extraction with EtOAc, and the organic layer was washed with saturated brine and dried over Na2SO4. The organic layer was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/EtOAc) to obtain 4-(5-bromopyridin-2-yl)morpholine (6.07 g).
後処理
- additionwas added
- concentrationThe reaction mixture was concentrated under reduced pressure, and water
- additionwas added to the residue
- extractionfollowed by extraction with EtOAc
- washthe organic layer was washed with saturated brine
- dry with materialdried over Na2SO4
- concentrationThe organic layer was concentrated under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography (hexane/EtOAc)
出典と根拠
- ORDレコード
- ord-bafc666d8c6c4fd09f3405f2b9654f78
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08716470B2
反応ノート
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