反应详情

Add hexane-2,5-dione (3.5 mL, 3.4 g, 30 2 mmol) to a solution of 5-bromo-4-trifluoromethyl-thiazol-2-ylamine hydrobromide (9.0 g, 27.4 mmol) in methanol (60 mL). Stir at room temperature overnight. Add phosphate buffer (50 mL, pH=7). Collect the resulting precipitate by filtration, washing with water. Dissolve the filter cake in CH2Cl2 and dry over sodium sulfate. Filter and concentrate under vacuum to obtain the title compound (8.2 g, 92%). 1H NMR (400 MHz, CDCl3) δ 5.91 (s, 2H), 2.27 (s, 6H).

1. customCollect the resulting precipitate
2. filtrationby filtration
3. washwashing with water
4. dissolutionDissolve the filter cake in CH2Cl2
5. dry with materialdry over sodium sulfate
6. filtrationFilter
7. concentrationconcentrate under vacuum