Acetic Anhydride → HCID 58371859、化合物
反応式
Cl.[Br:2][C:3]1[CH:13]=[CH:12][C:6]([C:7](=[NH:11])[NH:8][NH:9][CH3:10])=[CH:5][CH:4]=1.C(O[C:18](=O)[CH3:19])(=O)C>>[Br:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]2[N:11]=[C:18]([CH3:19])[N:9]([CH3:10])[N:8]=2)=[CH:12][CH:13]=1参加物
3
反応条件
- 温度
- 100 °C
実験手順
A mixture of 4-bromo-N′-methylbenzimidohydrazide hydrochloride 1 (1.7 g) (prepared according to a procedure in synthesis of Sch-1499895) in acetic anhydride (10 ml) was heated at 100° C. for 0.5 hour. After cooling and concentration under reduced pressure, the residue was dissolved in EtOAc, washed with saturated NaHCO3 twice, brine and dried (MgSO4). After evaporation of solvent, the residue was purified on silica gel. Elution with EtOAc gave 3-(4-bromophenyl)-1,5-dimethyl-1H-[1,2,4]-triazole 2BK (1.04 g).
後処理
- customprepared
- temperatureAfter cooling
- concentrationconcentration under reduced pressure
- dissolutionthe residue was dissolved in EtOAc
- washwashed with saturated NaHCO3 twice
- dry with materialbrine and dried (MgSO4)
- customAfter evaporation of solvent
- customthe residue was purified on silica gel
- washElution with EtOAc
出典と根拠
- ORDレコード
- ord-656f3ea274ec4f639a79657aad1623b9
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08716483B2
反応ノート
読み込み中…