반응 #340386

반응 방정식

4-trifluoromethyl-benzene-thioamide

ethyl-4-bromo-3-oxo-pentanoate

→

title compound

수율 47.2%

[5-Methyl-2-(4-trifluoromethyl-phenyl)-thiazol-4-yl]-acetic Acid Ethyl Ester

수율 47.2%

용매

ethanol

반응 조건

후처리

1. 1
   기타Seal this solution
2. 2
   온도Cool the resulting solution to room temperature
3. 3
   농축concentrate under reduced pressure
4. 4
   기타purify the residue
5. 5
   세척by flash chromatography (elute with 30% ethyl acetate/10% dichloromethane in heptane)

실험 절차

To a solution of 4-trifluoromethyl-benzene-thioamide (1.845 g, 9 mmol) in ethanol (15 mL, 200 proof) add ethyl-4-bromo-3-oxo-pentanoate (2.07 g, 9 mmol). Seal this solution warm the solution to 170° C. in a Personal Chemistry™ microwave oven and stir at this temperature for 20 min. Cool the resulting solution to room temperature, concentrate under reduced pressure and purify the residue by flash chromatography (elute with 30% ethyl acetate/10% dichloromethane in heptane) and obtain the title compound as a white solid (1.4 g). MS (ESI) m/z 330 (M+H); H1 NMR (CDCl3) δ1.87 (bs, 1H), 2.49 (s, 3H), 4.86 (s, 2H), 7.67 (d, J=8 Hz, 2H), 8.02 (d, J=8 Hz, 2H).

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