反应详情

2.0 g (14.6 mmol) methyl formylchloroacetate (A. Gangjee, A. Vidwans, E. Elzein, et. Al. J. Med. Chem. 2001, 44, 1993-2003), and 1.6 g (21.3 mmol) thioacetamide were dissolved in 10 ml water, heated, and reacted at 95° C. for 5 hr. The reaction product was extracted with ethyl acetate for 3 times, the ethyl acetate phases were combined, washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate, filtered, concentrated, and separated by a column chromatography to obtain 1.0 g methyl 2-methylthiazol-5-carboxylate (yield 43%), 1H NMR (CDCl3) 2.76 (3H, s), 3.89 (3H, s), 8.25 (1H, s).

1. temperatureheated
2. customreacted at 95° C. for 5 hr
3. extractionThe reaction product was extracted with ethyl acetate for 3 times
4. washwashed with a saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customseparated by a column chromatography