Hydrochloric Acid → HCID 21285560, compound

Participants

Reaction Conditions

Reaction Steps

The 3-amino-4'-dimethylaminobenzophenone may be prepared as follows: Stannous chloride in the dihydrate form (29.3 g) is added, at a temperature between 44° and 79° C., to a suspension of 4'-dimethylamino-3-nitrobenzophenone (11.4 g) in a mixture of concentrated hydrochloric acid (45 cc) and ethanol (120 cc), in the course of 35 minutes. The solution obtained is heated at a temperature in the vicinity of 79° C. for 3 hours. The suspension obtained is concentrated under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the vicinity of 50° C. The residue obtained is suspended in distilled water (350 cc) and an aqueous 10N sodium hydroxide solution (100 cc) is added, at a temperature in the vicinity of 5° C., to the suspension obtained and the mixture is stirred at a temperature in the vicinity of 20° C. for 30 minutes. The crystals formed are separated by filtration, washed 3 times with distilled water (60 cc in total) and air-dried. The crude product obtained is dissolved in boiling isopropanol (30 cc) and the solution obtained is cooled at a temperature in the vicinity of 4° C. for 2 hours. The crystals formed are separated by filtration, washed twice with isopropanol cooled to a temperature in the vicinity of 4° C. (20 cc in total) and twice with diethyl ether (40 cc) and then dried under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the vicinity of 20° C. in the presence of potassium hydroxide pellets. 3-amino-4'-dimethylaminobenzophenone (8.4 g) in the form of beige-coloured crystals, m.p. 110° C., is thereby obtained.

Provenance & Evidence