Thiomorpholine → 4-(5-Nitro-2-pyridinyl)thiomorpholine
反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[NH:11]1[CH2:16][CH2:15][S:14][CH2:13][CH2:12]1>O1CCCC1>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([N:11]2[CH2:16][CH2:15][S:14][CH2:13][CH2:12]2)=[N:3][CH:4]=1)([O-:10])=[O:9]参加物
4
実験手順
To a solution of 20 g (126 mmol) of 2-chloro-5-nitropyridine in 200 ml tetrahydrofuran were added dropwise 32.5 ml (315 mmol) thiomorpholine within 10 min. The reaction mixture was refluxed for additional 2 h. After cooling to room temperature, the solvent was removed in vacuo and the residue was re-dissolved in 200 ml ethyl acetate. The organic phase was washed with 200 ml 1 N sodium bicarbonate solution, dried (magnesium sulfate) and evaporated to give 29.3 g (quantitative) of the title compound as a yellow solid.
後処理
- temperatureThe reaction mixture was refluxed for additional 2 h
- customthe solvent was removed in vacuo
- dissolutionthe residue was re-dissolved in 200 ml ethyl acetate
- washThe organic phase was washed with 200 ml 1 N sodium bicarbonate solution
- dry with materialdried (magnesium sulfate)
- customevaporated
出典と根拠
- ORDレコード
- ord-0a6d260271f0483bbbb1796c2958fed9
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06849624B2
反応ノート
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