反应详情

A sulphonation flask is charged with 310 g 5-amino-4,6-dimethoxypyrimidin and 3500 ml dry CH2Cl2. To this mixture is added, within 15 minutes, a solution of 248.6 g chloroacetyl chloride in 400 ml dry CH2Cl2. The reaction is exothermic, the temperature rises from 14° to 32° and a suspension is formed. The reaction mixture is heated under reflux for 2 hours, then cooled to ambient temperature and evaporated till dryness. The solid residue is suspended in 3 l ice water, the suspension adjusted at pH 7-8 with diluted NaOH, cooled to 5° and sucked-off. The precipitate is washed twice with 500 ml ice water and then dried in vacuum at 60° to give the title compound, m.p. 193°-195°.

1. additionTo this mixture is added, within 15 minutes
2. customrises from 14° to 32°
3. customa suspension is formed
4. temperatureThe reaction mixture is heated
5. temperatureunder reflux for 2 hours
6. customevaporated till dryness
7. temperaturecooled to 5°
8. washThe precipitate is washed twice with 500 ml ice water
9. customdried in vacuum at 60°