反应详情

N-(4-Methyl-thiazol-2-yl)-acetamide (Example 17a) (4.0 g, 25.6 mmol) is dissolved in glacial acetic acid (100 ml) at room temperature. This solution is then treated portionwise with N-bromosuccinimide (4.6 g, 25.6 mmol). After 48 hours the reaction mixture is poured into water (1000 ml) and extracted with ethyl acetate (3×250 ml). The combined organic layers are washed with water (200 ml), brine (200 ml), dried over MgSO4, filtered and concentrated in vacuo. The residue is dissolved in toluene (100 ml) followed by the removal of the solvent in vacuo. This is repeated twice more and the resulting solid is dried in vacuo at 40° C. to give N-(5-bromo-4-methyl-thiazol-2-yl)-acetamide.

1. extractionextracted with ethyl acetate (3×250 ml)
2. washThe combined organic layers are washed with water (200 ml), brine (200 ml)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. dissolutionThe residue is dissolved in toluene (100 ml)
7. customfollowed by the removal of the solvent in vacuo
8. customthe resulting solid is dried in vacuo at 40° C.