HRID982471

反应详情

EQUATION

反应方程式

HRID 982471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of trans-2-[3-(2-oxopropylsulfonyl)-4-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 x), brine, dried, filtered, and evaporated to a residue, which was purified by preparative TLC (hexane-ethyl acetate; 7:3, v/v) to give the title compound: Rf 0.3; NMR (CDCl3) δ 2.38 (s, SO2CH2COCH3), 4.15 and 4.24 (2 t, OCH2CH2), 4.48 (s, SO2CH2), 5.22 (m, H-2 and H-5).

WORKUP

后处理

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