Ammonia → HCID 20071066, compound
Reaction equation
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]=1Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
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/cm2. After 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.
Workup
- temperatureThe reaction mixture is heated to 145°-150° C. for 12 hours
- temperatureAfter 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.
Sources & evidence
- ORD record
- ord-83c131031f14438284faf397fa7f4eb6
- Source dataset
- uspto-grants-1991_02
- Patent number
- US04992586
Reaction notes
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