1,3,5-Triazine → 1-(3-Nitrophenyl)-1H-1,2,4-triazole
반응식
Cl.[N+:2]([C:5]1[CH:6]=[C:7]([NH:11][NH2:12])[CH:8]=[CH:9][CH:10]=1)([O-:4])=[O:3].[N:13]1[CH:18]=NC=N[CH:14]=1.C(=O)(O)[O-].[Na+]>C(O)C>[N+:2]([C:5]1[CH:6]=[C:7]([N:11]2[CH:18]=[N:13][CH:14]=[N:12]2)[CH:8]=[CH:9][CH:10]=1)([O-:4])=[O:3]참가 물질
5
실험 절차
A mixture of 3-nitrophenylhydrazine hydrochloride (8.77 g) and 1,3,5-triazine (2.50 g) in ethanol (40 ml) was stirred under reflux for 4 hours. Then the mixture was poured into aqueous sodium bicarbonate and extracted with ethyl acetate twice. The combined organic phase was washed with aqueous sodium bicarbonate and brine, dried over magnesium sulfate and concentrated. The residue was chromatographed on silica gel column (hexane-ethyl acetate, 3:7) to give 1-(3-nitrophenyl)-1H-1,2,4-triazole (2.89 g) as a solid.
후처리
- temperatureunder reflux for 4 hours
- extractionextracted with ethyl acetate twice
- washThe combined organic phase was washed with aqueous sodium bicarbonate and brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customThe residue was chromatographed on silica gel column (hexane-ethyl acetate, 3:7)
출처 및 근거
- ORD 기록
- ord-a48fb3324bef49f8bf1c79a9431c2572
- 출처 데이터셋
- uspto-grants-2002_07
- 특허 번호
- US06426345B1
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