反应详情

温度

100 °C

To a nitrogen gas purged microwave vial of 2-(5-(5-chloro-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrrolo[2,3-b]pyridin-3-yl)pyridin-3-ylamino)-3-methyl-N-(2,2,2-trifluoroethyl)butanamide 2-1a (800 mg, 1.439 mmol), 2-DI-T-BUTYLPHOSPHINO-3,4,5,6-TETRAMETHYL-2′,4′,6′-TRI-I-PROPYLBIPHENYL (55.3 mg, 0.115 mmol) and Pd2 dba3 (26.3 mg, 0.029 mmol) in Dioxane (6 ml) was added 1 M KOH (4.32 ml, 4.32 mmol). The reaction mixture was sealed and heated in an oil bath at 100° C. for 18 h. The reaction was cooled, diluted with brine and product extracted with ethyl acetate. The organic extract was dried over sodium sulfate, filtered and concentrated to an oil. The oil was diluted with diethyl ether (18 ml) and sonicated. The resulting solid was filtered and washed with ether to give 720 mg white solid, 2-1b.

1. customThe reaction mixture was sealed
2. temperatureThe reaction was cooled
3. extractionextracted with ethyl acetate
4. extractionThe organic extract
5. dry with materialwas dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated to an oil
8. additionThe oil was diluted with diethyl ether (18 ml)
9. customsonicated
10. filtrationThe resulting solid was filtered
11. washwashed with ether