反应详情

To a solution of 2-amino-4-methoxy-7-phenyl-benzothiazole (200 mg, 0.67 mmol) in THF (10 m) was added DMAP (10 mg, 0.08 mmol), triethylamine (163 □l, 1.17 mmol) and 2-methoxybenzoyl chloride (136 □l, 1 mmol) in THF (2 ml). The mixture was then heated to reflux for 2 h, after cooling, it was partitioned between 1:1 AcOEt/THF (70 ml) and 5% NaHCO3 solution( 40 ml). The organic phase was washed with saturated NaCl solution (50 ml), dried with Na2SO4, filtered and the solvent removed under reduced presure. The residue was suspended in ether (10 ml), filtered, washed with ether then dried under vacuum (0.05 mmHg, 60° C.), to afford the title compound was a white solid (260 mg, 85% yield), MS: m/e=390.0 (M+).

1. temperatureThe mixture was then heated
2. temperatureto reflux for 2 h
3. temperatureafter cooling
4. customit was partitioned between 1:1 AcOEt/THF (70 ml) and 5% NaHCO3 solution( 40 ml)
5. washThe organic phase was washed with saturated NaCl solution (50 ml)
6. dry with materialdried with Na2SO4
7. filtrationfiltered
8. customthe solvent removed
9. filtrationfiltered
10. washwashed with ether
11. customthen dried under vacuum (0.05 mmHg, 60° C.)