反应详情

温度

0 °C

A mixture of 3-(5-bromothiophen-2-yl)-3-oxopropyl acetate (2.4 g, 8.8 mmol, 1 eq) in THF (150 ml) was stirred at 0° C., and NaBH4 (401.2 mg, 10.6 mmol, 2 eq) was added slowly and the reaction was stirred at 23° C. After 1 hour, Na2CO3.H2O was added. After 30 min the mixture was filtered and extracted with EtOAc (3×50 ml). The combined organic phases were washed (brine), dried (Na2SO4), filtered and concentrated to give a residue. The residue was purified by silica gel column chromatography (PE/EtOAc=5:1 as eluant) to give 3-(5-bromothiophen-2-yl)-3-hydroxypropyl acetate (1.92 g, 78.2%) as white solid. LC-MS (m/z)=279.1 [M+H]+

1. stirringthe reaction was stirred at 23° C
2. filtrationAfter 30 min the mixture was filtered
3. extractionextracted with EtOAc (3×50 ml)
4. washThe combined organic phases were washed (brine)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customto give a residue
9. customThe residue was purified by silica gel column chromatography (PE/EtOAc=5:1 as eluant)