反应详情

Tert-butyl(trans-3-(quinazolin-2-ylamino)cyclobutyl)carbamate, which was synthesized analagous to intermediate 10, (1.71 g, 5.44 mmol) was dissolved in dichloromethane (20 mL) and treated with trifluoroacetic acid (5 mL). The solution was stirred at room temperature for 20 minutes after which the solution was evaporated to dryness under reduced pressure. The crude oil was further dried under high vacuum then dissolved in dry dimethylsulfoxide (40 mL). 4,6-Dichloro-5-nitropyrimidine (1.5 g, 7.73 mmol) was added followed by potassium carbonate (1.8 g, 13.02 mmol) and the reaction heated at 60° C. After 2 hours the mixture was cooled and diluted with water (300 mL). The product precipitated out and was filtered off using a sintered glass frit. It was dried on the frit and used without purification.

1. customwas evaporated to dryness under reduced pressure
2. customThe crude oil was further dried under high vacuum
3. dissolutionthen dissolved in dry dimethylsulfoxide (40 mL)
4. temperaturethe reaction heated at 60° C
5. temperatureAfter 2 hours the mixture was cooled
6. customThe product precipitated out
7. filtrationwas filtered off
8. customIt was dried on the frit
9. customused without purification