Ammonia → HCID 20071066, compound

HRID 2291440Notes

Reaction equation

HRID 2291440 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]=1

Participants

5

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/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.

Workup

  1. temperatureThe reaction mixture is heated to 145°-150° C. for 12 hours
  2. temperaturecm2After cooling
  3. customthe expected product precipitates from the reaction mixture
  4. filtrationAfter being filtered off
  5. dry with materialit is dried hot under vacuum in the presence of phosphorus pentoxide
  6. customRecrystallized from isopropanol, it melts at 129° C.

Sources & evidence

ORD record
ord-6ee8bbc274d54ae2a2124e7f955928e8
Source dataset
uspto-grants-1989_01
Patent number
US04797129

Reaction notes

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