反应详情

温度

60 °C

Dimethylcarbamoyl chloride (7.5 grams, 0.07 mole) was added to a solution of 3-aminobenzophenone (10 grams, 0.05 mole) in dimethylformamide (150 ml.), triethylamine (10 ml.) at 10° C. with stirring and ice cooling. The reaction temperature was next raised to 60° C. for 20 hours, then cooled and poured onto ice water (500 grams) containing dilute hydrochloric acid. A tarry solid was obtained by decanting off the aqueous organic solution. Purification was effected by dissolving the tarry solid in methylene chloride and passing through a silica gel dry column eluant methylene chloride. On elution with dichloromethane, the product, 3-(m-benzoylphenyl)-1,1-dimethyl urea, is obtained. Melting point was 104° -105° C. Crystallization from benzene-hexane (9:1) mixture gave solid 109° - 110° C., which on benzene-hexane crystallizations afforded a melting point of from 121° to 122° C. identified as the desired urea by comparison with the sample prepared from phosgene and dimethylamine.

1. temperaturecooled
2. additionpoured onto ice water (500 grams)
3. customA tarry solid was obtained
4. customby decanting off the aqueous organic solution
5. customPurification
6. dissolutionby dissolving the tarry solid in methylene chloride
7. dry with materialdry column eluant methylene chloride
8. washOn elution with dichloromethane