反应详情

A mixture of Example 81C (400 mg, 1 mmol), 1-mercaptopropan-2-ol (277 mg, 3 mmol) and potassium carbonate (415 mg, 3 mmol) in DMF (10 mL) was heated at 50° C. for 16 hours. The mixture was then poured into water and extracted with ethyl acetate. The acetate layer was washed with brine, dried with MgSO4, filtered, and concentrated under reduced pressure. Purification by chromatography afforded 320 mg of the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 0.91 (t, J=7.3 Hz, 3H), 1.15-1.24 (m, 3H), 1.27-1.44 (m, 11H), 1.54-1.79 (m, 2H), 2.68-3.07 (m, 2H), 3.76-3.94 (m, 4H), 4.27-4.45 (m, 2H), 4.94 (d, J=4.8 Hz, 1H), 6.83 (s, 1H), 7.42-7.52 (m, 1H), 7.54-7.66 (m, 1H), 8.24 (d, J=1.6 Hz, 1H). MS (DCI/NH3) m/z 472 (M+H)+. Anal. calculated for C23H32F3N3O2S: C, 58.58 H, 6.84 N, 8.91. Found: C, 58.57 H, 6.96 N, 8.77.

1. extractionextracted with ethyl acetate
2. washThe acetate layer was washed with brine
3. dry with materialdried with MgSO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customPurification by chromatography