反应详情

A mixture of Example 6C (400 mg, 0.97 mmol) and dimethyl sulfate (0.37 mL, 3.88 mmol) in toluene (2 mL) was heated in a microwave reactor (300 W, CEM Explorer®) at 150° C. for 1 hour. The solvent was removed under reduced pressure and the residue was purified by flash chromatography (silica gel; solvent A=EtOAc/MeOH/Et3N (90:10:0.5); solvent B=hexane in 10-60% gradient A/B) to yield 331.5 mg (80%) of the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.44 (s, 9H), 1.50-1.67 (m, 1H), 1.75-1.96 (m, 2H), 1.99-2.14 (m, 1H), 3.64-3.84 (m, 2H), 4.12 (s, 3H), 4.18-4.26 (m, 1H), 4.55-4.77 (m, 2H), 6.98 (s, 1H), 7.63 (t, J=7.73 Hz, 1H), 8.00-8.13 (m, 2H); MS (ESI) m/z 428 (M+1H).

1. customThe solvent was removed under reduced pressure
2. customthe residue was purified by flash chromatography (silica gel