HCID 3106275, 화합물 → 3,5-Dinitropyridine
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[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].C(O)=O.C=O>CO.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]참가 물질
5
실험 절차
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, 300MHz) δ: 9.77 (m, 2H), 9.27 (m, 1H).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-6ff30fc9ce5c4ac4b557e3ed9a283134
- 출처 데이터셋
- uspto-grants-1999_06
- 특허 번호
- US05914328
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