反应详情

A mixture of Example 1A (15.5 g, 0.1 mol), 2-bromothiazole (18.2 g, 0.11 mol) and potassium carbonate (15.2 g, 0.11 mol) in dimethylsulfoxide was heated at 160° C. under nitrogen for 6 hours. It was then cooled and treated with water, and the aqueous phase was extracted with methylene chloride. The organic layer washed with brine, dried (MgSO4) and concentrated to give 27.5 g of the crude material which was purified on silica gel (5˜35% ethyl acetate in hexane) to afford 21.5 g of the title compound (91% yield) 1H NMR (500 MHz, CDCl3) δ ppm 1.32-1.36 (m, 6 H) 1.34 (none, 6 H) 1.34 (none, 5 H) 4.45-4.57 (m, 1 H) 6.76 (d, J=3.91 Hz, 1 H) 6.87-6.93 (m, 2 H) 7.15-7.20 (m, 2 H) 7.21 (d, J=3.91 Hz, 1 H). MS (ESI): m/z 236 (M−H).

1. temperatureIt was then cooled
2. extractionthe aqueous phase was extracted with methylene chloride
3. washThe organic layer washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customto give 27.5 g of the crude material which
7. customwas purified on silica gel (5˜35% ethyl acetate in hexane)