反应详情

温度

0 °C

Trimethylaluminium (2M in hexanes)(0.551 mL, 1.10 mmol) was added to 5-chloropyridin-2-amine (135 mg, 1.05 mmol) in toluene (8 mL) cooled to 0° C. under nitrogen. The resulting solution was stirred at 0° C. for 20 minutes. (2S)-methyl 3-((S)-1-(tert-butyldimethylsilyloxy)propan-2-yloxy)-2-(1-(3-chloropyridin-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)propanoate (Intermediate AO2) (500 mg, 0.96 mmol) in toluene (8 mL) was added and the reaction was heated to 100° C. for 5 hours in the microwave reactor. The reaction was allowed to cool to room temperature before adding EtOAc (30 mL) and 20% sodium potassium tartrate solution (30 mL), which was stirred vigorously for 16 hours. The phases were separated and the organic layer was washed with sat. brine (15 mL), dried (MgSO4) and evaporated to give crude product (300 mg) that was used without further purification. m/z (ES+), (M+H)+=618.44; HPLC tR=23.55 min

1. temperaturethe reaction was heated to 100° C. for 5 hours in the microwave reactor
2. temperatureto cool to room temperature
3. stirringwas stirred vigorously for 16 hours
4. customThe phases were separated
5. washthe organic layer was washed with sat. brine (15 mL)
6. dry with materialdried (MgSO4)
7. customevaporated