HCID 3106275、化合物 → 3,5-Dinitropyridine
反応式
[N+:1]([C:4]1[C:5](NN)=[N:6][CH:7]=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1)([O-:3])=[O:2]>CO.O.C([O-])(=O)C.[Ag+]>[N+:10]([C:8]1[CH:7]=[N:6][CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:9]=1)([O-:12])=[O:11]参加物
4
実験手順
Silver acetate (2.0 g) was added to a solution of the crude 3,5-dinitro-pyridinyl-hydrazine (2.2 g) in a mixture of methanol:H2O (1:1, 6 ml), and the mixture was stirred at reflux overnight. Solvent was evaporated, then water and conc. NH4OH were added. The mixture was extracted with ethyl ether, the combined extracts were dried over MgSO4, concentrated and purified by column chromatography (5:1 hexane: ethyl acetate) to give the title compound (400 mg) in 21.8% yield. MS (DCI/NH3) m/e: 124 (M-46+1). 1H NMR (CDCl3, 300 MHz) δ: 9.77 (m, 2H), 9.27 (m, 1H).
後処理
- temperatureat reflux overnight
- customSolvent was evaporated
- additionwater and conc. NH4OH were added
- extractionThe mixture was extracted with ethyl ether
- dry with materialthe combined extracts were dried over MgSO4
- concentrationconcentrated
- custompurified by column chromatography (5:1 hexane: ethyl acetate)
出典と根拠
- ORDレコード
- ord-25ca1739e32740e497785605c05b1fd6
- 出典データセット
- uspto-grants-1999_09
- 特許番号
- US05948793
反応ノート
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