Sodium Hydroxide → HCID 18182237、化合物
反応式
[C:1]([C:9]1[CH:14]=[CH:13][N+:12]([O-])=[CH:11][CH:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:18])=O.[OH-].[Na+]>O>[C:1]([C:9]1[CH:14]=[CH:13][N:12]=[C:11]([Cl:18])[CH:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
5
実験手順
A mixture of 2.5 g 4-benzoylpyridine N-oxide m.p. 127°-30° C. (obtained according to T. KATO et. al., Yakugaku Zasshi 86, 1022-26, 1966), and 6 ml phosphorus oxychloride is refluxed for 2 hrs. After cooling, the reaction mixture is very slowly added to ice: water, basified (10N NaOH) and extracted with methylene chloride. The organic layer is washed with water, dried and solvent removed in a rotary evaporator. Yield: 2.4 g of title product, identical with that described in Ex. 4.
後処理
- temperatureis refluxed for 2 hrs
- temperatureAfter cooling
- additionthe reaction mixture is very slowly added to ice
- extractionextracted with methylene chloride
- washThe organic layer is washed with water
- customdried
- customsolvent removed in a rotary evaporator
出典と根拠
- ORDレコード
- ord-69eaac4647914a1e80fab826874a6c33
- 出典データセット
- uspto-grants-1986_09
- 特許番号
- US04614833
反応ノート
読み込み中…