反应详情

温度

22 °C

The product of step h) (948 mg, 3.35 mmol) in dichloroethane (17 ml) was treated with K2CO3 (1.85 g, 13.4 mmol) and Ace-Cl (1.45 ml, 13.4 mmol) at 80° C. for 16 hours. Next, the reaction mixture was filtered, concentrated and the residue was dissolved in anhydrous MeOH (25 ml) and stirred for 1 hour at 22° C. The MeOH was concentrated and triturated with ether producing 733 mg (95%) of the subtitle compound. 1H NMR (300 MHz, d6-DMSO, ppm) 1.27 (d, J=7 Hz, 3H); 2.97-3.10 (m, 1H); 3.19-3.38 (m, 2H); 3.42-3.62 (m, 3H); 3.78-3.88 (m, 1H); 6.92 (d, J=5 Hz, 1H); 7.47 (d, J=5 Hz, 1H); 9.05 (br s, 1H); 9.38 (br s, 1H); MS calculated for C11H15NS+H 194, observed 194.

1. filtrationNext, the reaction mixture was filtered
2. concentrationconcentrated
3. dissolutionthe residue was dissolved in anhydrous MeOH (25 ml)
4. concentrationThe MeOH was concentrated
5. customtriturated with ether producing 733 mg (95%) of the subtitle compound