反应详情

A mixture of 2-(2-diisopropylaminoethylamino)-4,6-dimethyl pyrimidine (17.0 g. 0.068 mole) and sodium hydride (50% in mineral oil) (4.19 g., 0.86 mole) in 175 ml. of dry toluene is stirred under nitrogen at 85°-95° C. for one half hour and then heated under reflux for one half hour. Dimethylcarbamoyl chloride (8.6 g., 0.08 mole) is added and heating under reflux is continued for twenty-four hours. The reaction is cooled and ethanol (10 ml) and sodium hydroxide (75 ml., 3.3N) are added. The aqueous layer is extracted with methylene chloride and the extracts are dried over sodium sulfate and concentrated to an oil. The oil is distilled at 0.5 mm of Hg and the product boiling at 155°-158° C. is collected.

1. temperatureheated
2. temperatureunder reflux for one half hour
3. temperatureheating
4. temperatureunder reflux
5. waitis continued for twenty-four hours
6. temperatureThe reaction is cooled
7. extractionThe aqueous layer is extracted with methylene chloride
8. dry with materialthe extracts are dried over sodium sulfate
9. concentrationconcentrated to an oil
10. distillationThe oil is distilled at 0.5 mm of Hg
11. customthe product boiling at 155°-158° C. is collected