反应详情

The mixture of crude 5-(4-(1-acetyl-5-cyclopropyl-1H-pyrazol-3-ylamino)-5-bromopyrimidin-2-yl)-N-(2-(dimethylamino)ethyl)thiophene-2-sulfonamide (from step 4), Pd(PPh3)2Cl2 (14 mg, 0.02 mmol, 0.05 eq) and CuI (8 mg, 0.04 mmol, 0.1 eq) was flushed with nitrogen. Anhydrous THF (12 mL) and Et3N (121 mg, 1.2 mmol, 3.0 eq) were added and the reaction mixture was flushed with nitrogen. Ethynyl-trimethylsilane (118 mg, 1.2 mmol, 3.0 eq) was added and the reaction mixture was stirred at rt for 1 h. Then, the reaction mixture was concentrated to about 5 mL, which was taken in EtOAc and was washed with water, brine. The combined organic layers were concentrated to afford crude 5-(4-(1-acetyl-5-cyclopropyl-1H-pyrazol-3-ylamino)-5-((trimethylsilyl)ethynyl)pyrimidin-2-yl)-N-(2-(dimethylamino)ethyl) thiophene-2-sulfonamide, which was used for the next step without further purification). LC-MS (m/z)=572.0 [M+H]+

1. customwas flushed with nitrogen
2. customthe reaction mixture was flushed with nitrogen
3. concentrationThen, the reaction mixture was concentrated to about 5 mL, which
4. washwas washed with water, brine
5. concentrationThe combined organic layers were concentrated