反应详情

To a sealed microwave reaction vessel containing methyl 2-(6-chloropyridin-3-yl)acetate (200 mg, 1.08 mmol), 3,3-difluoroazetidine hydrochloride (154 mg, 1.19 mmol), Xantphos (93 mg, 0.162 mmol), Cs2CO3 (1.054 g, 3.23 mmol), and Pd2(dba)3 (99.0 mg, 0.11 mmol) was added 3.0 ml of dioxane. The reaction mixture was microwave radiated at 90 C for 60.0 min. It was cooled to room temperature and diluted with CH2Cl2 (20.0 ml). The suspension was filtered, washed with CH2Cl2 (3×10.0 ml), and the filtrate was washed with water and brine. The organic layer was dried over anhydrous Na2SO4, filtered. The filtrate was concentrated. The residue was purified by a standard method to give the title compound.

1. filtrationThe suspension was filtered
2. washwashed with CH2Cl2 (3×10.0 ml)
3. washthe filtrate was washed with water and brine
4. dry with materialThe organic layer was dried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationThe filtrate was concentrated
7. customThe residue was purified by a standard method