反应详情

温度

160 °C

Methyl 3-hydroxy-5-[(3S)-tetrahydrofuran-3-yloxy]benzoate (875 mg, 3.68 mmol), 2-(azetidin-1-ylcarbonyl)-5-bromopyridine (1.06 g, 4.41 mmol), caesium carbonate (3.59 g, 11.03 mmol), and bromotris(triphenylphosphine)copper (0.69 g, 0.735 mmol) were added together in DMA (16 mL) and heated in a microwave reactor at 160° C. for 9 hours. The mixture was taken up in water (25 mL) and washed with ethyl acetate (2×20 mL). The aqueous layer was acidified with 1N hydrochloric acid (30 mL) and extracted with ethyl acetate (5×30 mL). The combined organic extract was washed with water (30 mL), brine (30 mL), dried (MgSO4), filtered and evaporated to give a brown solid which was triturated with diethyl ether to give the desired compound as a beige solid (820 mg).

1. washwashed with ethyl acetate (2×20 mL)
2. extractionextracted with ethyl acetate (5×30 mL)
3. extractionThe combined organic extract
4. washwas washed with water (30 mL), brine (30 mL)
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. customto give a brown solid which
9. customwas triturated with diethyl ether