反应详情

温度

100 °C

A mixture of ethyl 3-bromo-4-oxopentanoate (2 g, 8.98 mmol, 1 eq), and 4-(3-chloropropoxy)benzenecarbothioamide ax71 (2.06 g, 8.97 mmol, 1 eq) in dimethylformamide (4 ml) is stirred at 100° C. for 2 h. The reaction mixture is then added to ethyl acetate (200 ml) and the precipitate filtered off. The organic layer is washed with water (4×100 ml), brine, dried over magnesium sulfate and filtered. The solvent is removed under reduced pressure. Purification by chromatography over silicagel (eluent: benzine/ethyl acetate 95:5 to 85:15) affords 1.3 g of ethyl {2-[4-(3-chloropropoxy)phenyl]-4-methyl-1,3-thiazol-5-yl}acetate i102.

1. filtrationthe precipitate filtered off
2. washThe organic layer is washed with water (4×100 ml), brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customThe solvent is removed under reduced pressure
6. customPurification by chromatography over silicagel (eluent: benzine/ethyl acetate 95:5 to 85:15)