反应详情

0.18 g (0.04 equivalent) of Pd(PPh3)4 and then 1.2 g (0.0084 mol) of 5-chloro-2-thiopheneboronic acid are added to a solution of 1.4 g (0.0038 mol) of ethyl 2-[(4-bromophenyl)oxy]-4-cyclohex-1-en-1-ylbutanoate in 20 ml of dimethoxyethane. 4.2 ml of 2M sodium carbonate solution are added at room temperature. The reaction mixture is stirred overnight and then refluxed for 2 hours. After cooling to room temperature, the mixture is taken up in water and extracted with ethyl acetate. The extract is washed with 1N sodium hydroxide and then with saturated aqueous NaCl solution and finally dried over Na2SO4. After concentrating, the black oil obtained is purified by flash chromatography (95/5 heptane/ethyl acetate). 1.1 g of a thick oil are obtained.

1. temperaturerefluxed for 2 hours
2. extractionextracted with ethyl acetate
3. washThe extract is washed with 1N sodium hydroxide
4. dry with materialwith saturated aqueous NaCl solution and finally dried over Na2SO4
5. concentrationAfter concentrating
6. customthe black oil obtained
7. customis purified by flash chromatography (95/5 heptane/ethyl acetate)