反应详情

温度

150 °C

To a microwave vial was added 6-trifluoromethoxy-2H-chromene-3-carbonitrile (100 mg, 0.4 mmol) and 10 M of sodium hydroxide in water (2 mL, 20 mmol). The reaction mixture was heated at 150° C. for 10 minutes in the microwave. The reaction mixture was acidified with conc. HCl then extracted with EtOAc (3×30 mL). The combined organics were washed with brine (3×30 mL), dried (MgSO4), filtered and concentrated, to give the product (42 mg) as a solid. m/z=258.9 (M−1), r.t.=3.43 mins. 1H NMR (400 MHz; CDCl3) δ 7.50 (1H, s), 7.11 (1H, dd), 7.04 (1H, d), 6.84 (111, d), 5.02 (2H, d).

1. extractionthen extracted with EtOAc (3×30 mL)
2. washThe combined organics were washed with brine (3×30 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated