反应详情

温度

110 °C

Z2—S-methyl isothiourea (0.097 g, 0.27 mmol) was added to the methyl ester of Example 35j (0.1 g, 0.27 mmol) in dry DMF (8 mL) and the reaction mixture was heated at 110° C. for 2 h. It was treated with water and extracted with ethyl acetate. The ethyl acetate layer was concentrated and the solid obtained was purified using flash chromatography (silica gel, EtOAc/PE60-80° C.). The product obtained was then subjected to hydrolysis as described in Example 1i to obtain the title compound. Yield: 26.22%; 1H NMR (DMSO-d6): δ 2.60 (s, 3H, CH3), 5.20 (s, 2H, CH2), 5.30 (s, 2H, SO2—CH2), 7.35 (m, 5H, Ar), 7.70 (s, 2H, Ar), 8.10 (d, 2H, Ar); MS: m/e (EI+) 529 (M+).

1. extractionextracted with ethyl acetate
2. concentrationThe ethyl acetate layer was concentrated
3. customthe solid obtained
4. customwas purified
5. customflash chromatography (silica gel, EtOAc/PE60-80° C.)
6. customThe product obtained
7. customwas then subjected to hydrolysis