反应详情

温度

22 °C

The product from step g) (605 mg, 1.46 mmol) in dichloroethane (7 ml) was treated with powdered K2CO3 (806 mg, 5.84 mmol) and 1-chloroethyl chloroformate (Ace-Cl) (632 μl, 5.84 mmol) at 80° C. for 16 hours. Next, the reaction was cooled, filtered and concentrated providing an oily residue. This oily residue was diluted with anhydrous MeOH (15 ml) and stirred for 1 hour at 22° C. The solvent was concentrated and the crude residue was purified by preparative LC/MS providing title compound. 1H NMR (300 MHz, CD3OD, ppm) 2.65-2.75 (m, 1H); 3.05-3.30 (m, 2H); 3.32-3.80 (m, 4H); 4.10-4.28 (br m, 1H); MS calculated for C9H9Br2NS+H 324, observed 322, 324, 326.

1. temperatureNext, the reaction was cooled
2. filtrationfiltered
3. concentrationconcentrated
4. customproviding an oily residue
5. concentrationThe solvent was concentrated
6. customthe crude residue was purified by preparative LC/MS