Pyridine → HCID 22141268、化合物
反応式
O[CH:2]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[CH:6]=1)[C:3]#[N:4].N1C=CC=CC=1.S(Cl)([Cl:22])=O>C(OCC)C>[Cl:22][CH:2]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[CH:6]=1)[C:3]#[N:4]参加物
5
実験手順
A solution of 2-hydroxy-2-(3-nitrophenyl)acetonitrile (Preparation 113, 1.0 g, 5.62 mmol) in diethyl ether (10 ml) was stirred at room temperature and treated with pyridine (0.1 ml, 1.24 mmol) followed by thionyl chloride (0.82 ml, 11.2 mmol) dropwise over 5 minutes. The mixture was gently heated under reflux and after 30 min the solvent was removed by evaporation to give a pale yellow solid. This was purified by column chromatography on silica gel eluting with hexane:ethyl acetate (3:1 and then 2:1) to give the title compound as a white crystalline solid (980 mg, 89%).
後処理
- temperatureThe mixture was gently heated
- temperatureunder reflux and after 30 min the solvent
- customwas removed by evaporation
- customto give a pale yellow solid
- customThis was purified by column chromatography on silica gel eluting with hexane:ethyl acetate (3:1
出典と根拠
- ORDレコード
- ord-7c0a6bca5b5b4ced8c0ae0fd1dd0403a
- 出典データセット
- uspto-grants-2006_05
- 特許番号
- US07049444B2
反応ノート
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