反应详情

温度

80 °C

A mixture of trans-2-[3-(2-oxopropylsulfonyl)-4-n-propoxy-5-hydroxyphenyl]-5-(3,4,5-trimethoxyphenyl)tetrahydrofuran (30 mg, 0.059 mmol), 3-bromo-1-propanol (12 uL, 0.13 mmol) and potassium carbonate (17 mg, 0.12 mmol) in DMF (0.5 mL) was heated at 80° C. with stirring under nitrogen for 1 h. The reaction mixture was cooled and diluted with ethyl ether. It was washed with water (2×), brine, dried, filtered, and evaporated to a residue (33 mg), which was purified by preparative TLC (hexane ethyl acetate; 7:3, v/v) to give the title compound (20 mg, 61%): Rf 0.3; NMR (CDCl3) δ 2.38 (s, SO2CH2COCH3), 4.15 & 4.24 (2 t, OCH2CH2), 4.48 (s, SO2CH2), 5.22 (m, H-2 & H-5).

1. temperatureThe reaction mixture was cooled
2. washIt was washed with water (2×), brine
3. customdried
4. filtrationfiltered
5. customevaporated to a residue (33 mg), which
6. customwas purified by preparative TLC (hexane ethyl acetate