反应详情

4,6-Dichloro-5-nitropyrimidine (8.88 g) is dissolved in 400 ml of methylene chloride and cooled to -78°. Then triethylamine (6.7 ml) and 1-benzyl-4-N-ethylaminopiperidine (EXAMPLE 205, 10.00 g) is added and the reaction is stirred 1 hr at -78° and slowly warmed to 20°-25°. The reaction is poured into saturated aqueous sodium bicarbonate, extracted with methylene chloride, washed with saline, dried and concentrated under reduced pressure. Purification by flash column chromatography (10% ethyl acetate/hexane to 50% ethyl acetate/hexane) gives the title compound.

1. temperaturecooled to -78°
2. temperatureslowly warmed to 20°-25°
3. extractionextracted with methylene chloride
4. washwashed with saline
5. customdried
6. concentrationconcentrated under reduced pressure
7. customPurification by flash column chromatography (10% ethyl acetate/hexane to 50% ethyl acetate/hexane)