反应详情

温度

150 °C

To a solution of (cis) (4-(4-chloroindolin-1-yl)thiazol-2-yl) (2,6-dimethylmorpholino) methanone (Step-2, of compound 45, 0.6 g, 1.59 mmol in dimethyl acetamide (10 ml) were added 4-bromobenzenesulfonamide (0.41 g, 1.75 mmol) and potassium acetate (0.31 g, 3.18 mmol) at 25° C. in a tube, the nitrogen gas was bubbled through reaction mixture for 15 minutes. To this was added palladium (II) acetate (0.03 g, 0.16 mmol) under nitrogen and the tube was sealed. The reaction mixture was heated at 150° C. for 18 hr under stirring. The progress of reaction was monitored by TLC. The reaction mixture was cooled to 25° C. and concentrated under reduced pressure. The residue was dissolved in ethyl acetate (30 ml), reaction mixture was washed with water (2×10 ml), dried over sodium sulphate and concentrated under reduced pressure to obtain a crude product; which was purified by preparative HPLC to obtain the title compound (0.22 g, 26.0%). MS: m/z 533 (M+1).

1. customthe nitrogen gas was bubbled through reaction mixture for 15 minutes
2. customthe tube was sealed
3. customThe progress of reaction
4. temperatureThe reaction mixture was cooled to 25° C.
5. concentrationconcentrated under reduced pressure
6. dissolutionThe residue was dissolved in ethyl acetate (30 ml)
7. customreaction mixture
8. washwas washed with water (2×10 ml)
9. dry with materialdried over sodium sulphate
10. concentrationconcentrated under reduced pressure
11. customto obtain a crude product
12. customwhich was purified by preparative HPLC