反应详情

A mixture of 3-chloro-4-fluoro-7-methoxy-1-benzothiophene-2-carboxylic acid (1.09 g, 4.19 mmol) and diazobicycloundecane (DBU) (2 mL) in dimethylacetamide (15 mL) was heated in a sealed vessel in a microwave (300 W, 100%) for 1 h. After cooling to room temperature the mixture was diluted with diethyl ether (100 mL) and washed with brine (2×100 mL). The organic phase was dried (MgSO4) and the solvent removed in vacuo. The residue was purified by flash chromatography eluting silica gel with hexane:diethyl ether [10:1] to yield a white solid (520 mg, 57%); δH (300 MHz, CDCl3) 7.24 (1H, s, Ar), 7.05–6.92 (1H, m, Ar), 6.70–6.60 (1H, dd, Ar), 3.96 (3H, s, OCH3).

1. temperaturewas heated in a sealed vessel in a microwave (300 W, 100%) for 1 h
2. washwashed with brine (2×100 mL)
3. dry with materialThe organic phase was dried (MgSO4)
4. customthe solvent removed in vacuo
5. customThe residue was purified by flash chromatography
6. washeluting silica gel with hexane