反应详情

A mixture of 2,6-dichloro-3-[N-(phthalimidoacetyl)-N-methylamino]toluene (303 mg), N-bromosuccinimide (150 mg), 2,2'-azobis-(2,4-dimethyl-4-methoxyvaleronitrile) (30 mg) and dichloromethane (6 ml) was heated under reflux for 5 hours. N-Bromosuccinimide (75 mg) was added therein and the mixture was heated under reflux for additional 3 hours. The reaction mixture was washed with saturated sodium bicarbonate solution twice and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was crystallized from diethyl ether to give 3-bromomethyl-2,4-dichloro-N-methyl-N-(phthalimidoacetyl)aniline (102 mg) as crystals. mp: 211° C. (dec.)

1. temperaturewas heated
2. temperatureunder reflux for 5 hours
3. temperaturethe mixture was heated
4. temperatureunder reflux for additional 3 hours
5. washThe reaction mixture was washed with saturated sodium bicarbonate solution twice
6. dry with materialbrine, dried over magnesium sulfate
7. customevaporated in vacuo
8. customThe residue was crystallized from diethyl ether