反应详情

A solution of Intermediate 2-chloro-4-(3-iodo-1-isopropyl-1H-pyrazol-4-yl)pyrimidine (1.4 g, 4.01 mmol), (S)-methyl 1-aminopropan-2-ylcarbamate (0.8 g, 6 mmol) and triethylamine (2.8 ml, 20 mmol) in isopropanol (30 ml) and dioxane (20 mL) was heated in a sealed vessel at 125° C. for 48 hours. The cooled mixture was concentrated under vacuum, and aqueous sodium bicarbonate was added to the residue. The mixture was extracted with ethyl acetate, and the combined extracts were dried over sodium sulfate, filtered, and concentrated. The crude residue was purified by silica gel column chromatography (1:2 hexanes/ethyl acetate eluant) to provide the title compound as a white solid. MS m/z 445.0 (M+1).

1. concentrationThe cooled mixture was concentrated under vacuum, and aqueous sodium bicarbonate
2. additionwas added to the residue
3. extractionThe mixture was extracted with ethyl acetate
4. dry with materialthe combined extracts were dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude residue was purified by silica gel column chromatography (1:2 hexanes/ethyl acetate eluant)