反应详情

温度

0 °C

A suspension of (E)-3-(4-bromo-thiophen-2-yl)-acrylic acid (3.0 g, 12.9 mmol) in anhydrous acetone (20 ml) was cooled in an ice-bath to 0° C. and treated with triethylamine (2.15 ml, 15.4 mmol) and ethyl chloroformate (1.24 ml, 15.4 mmol). The reaction was left to stir for 0.5 h before being treated with a solution of sodium azide (1.0 g, 15.4 mmol) in distilled water (4 ml). After stirring for 1 h at 0° C., the reaction was further diluted with distilled water (40 ml) and extracted with DCM (3×25 ml). The organic layer was dried (MgSO4) and filtered for direct use in the next reaction.

1. waitThe reaction was left
2. stirringAfter stirring for 1 h at 0° C.
3. extractionextracted with DCM (3×25 ml)
4. dry with materialThe organic layer was dried (MgSO4)
5. filtrationfiltered for direct use in the next reaction