反应详情

A solution of 1 g (5.58×10−3 moles) of 5-nitrobenzo[b]thiophene and 0.65 ml (6.64×10−3 moles) of 2-chloropropionyl chloride dissolved in 40 ml of dry chloroform was added dropwise over 650 mg of aluminum trichloride, dissolved in 20 ml dry chloroform under a nitrogen atmosphere. The mixture was left to react for 24 hours at room temperature and an additional amount of 650 mg of aluminum trichloride and 0.65 ml of 2-chloropropionyl chloride was added. After 48 hours reaction 100 ml of HCl 1.5N were added, followed by decantation and the organic phase was subsequently washed with a dilute solution of NaHCO3, with H2O and with a saturated solution of NaCl. It was dried with Na2SO4, the solvent was removed and it was purified in a silica column using hexane/toluene (25:75) as mobile phase. Yield: 30%.

1. waitThe mixture was left
2. customto react for 24 hours at room temperature
3. additionwere added
4. washthe organic phase was subsequently washed with a dilute solution of NaHCO3, with H2O and with a saturated solution of NaCl
5. dry with materialIt was dried with Na2SO4
6. customthe solvent was removed
7. customit was purified in a silica column