Ammonia → HCID 20071066、化合物
反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([NH:9][CH3:10])[C:3]=1[N+:11]([O-:13])=[O:12].[NH3:14]>O.C(O)C>[Cl:8][C:6]1[CH:5]=[C:4]([NH:9][CH3:10])[C:3]([N+:11]([O-:13])=[O:12])=[C:2]([NH2:14])[CH:7]=1参加物
5
実験手順
0.034 mole (7.5 g) of 2,4-dichloro-6-methylaminonitrobenzene is added in an autoclave to 100 ml of a 28% strength solution of ammonia in water and 50 ml of ethanol. The reaction mixture is heated to 145°-150° C. for 12 hours, the pressure being 12 kg/cm2After cooling, the expected product precipitates from the reaction mixture. After being filtered off and reslurried in water, it is dried hot under vacuum in the presence of phosphorus pentoxide. Recrystallized from isopropanol, it melts at 129° C.
後処理
- temperatureThe reaction mixture is heated to 145°-150° C. for 12 hours
- temperaturecm2After cooling
- customthe expected product precipitates from the reaction mixture
- filtrationAfter being filtered off
- dry with materialit is dried hot under vacuum in the presence of phosphorus pentoxide
- customRecrystallized from isopropanol, it melts at 129° C.
出典と根拠
- ORDレコード
- ord-6ee8bbc274d54ae2a2124e7f955928e8
- 出典データセット
- uspto-grants-1989_01
- 特許番号
- US04797129
反応ノート
読み込み中…