反应详情

2.5 g (10.4 mmol) of 3-chloro-2-methoxycarbonyl-6-methylbenzo[b]thiophene (prepared according to J. Org. Chem. 41, 3399 (1976)) are boiled under reflux in 150 ml of chlorobenzene with 1.87 g of NBS and 420 mg of dibenzoyl peroxide for 5 h. After distilling off the chlorobenzene in a rotary evaporator, the residue obtained is taken up in EA, and the EA solution is washed with satd. NaHCO3 solution, 10% strength Na2SO3 solution and satd. NaCl solution, dried over Na2SO4 and concentrated. Chromatography on SiO2 using EA/Hep 1:20 yields 2.28 g of the title compound.

1. distillationAfter distilling off the chlorobenzene
2. customin a rotary evaporator
3. customthe residue obtained
4. washthe EA solution is washed with satd
5. dry with materialNaCl solution, dried over Na2SO4
6. concentrationconcentrated