1,3,5-Triazine → 1-(3-Nitrophenyl)-1H-1,2,4-triazole
反応式
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]参加物
5
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-cc6b3a560c9b40168ddbcd3fe480e95b
- 出典データセット
- uspto-grants-2004_04
- 特許番号
- US06727245B2
反応ノート
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