HRID1181137

反应详情

EQUATION

反应方程式

HRID 1181137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A 25 mL round bottomed flask under a nitrogen atmosphere was charged with toluene-4-sulfonic acid 2-(5-methyl-2-phenyloxazol-4-yl)ethyl ester (0.77 g, 2.17 mmol), 2-(4-hydroxy-2-hydroxymethylphenoxy)-2-methylpropionic acid ethyl ester (0.5 g, 1.97 mmol), and absolute ethanol (10 mL). Potassium carbonate (0.54 g, 3.94 mmol, 325 mesh) was added, and the reaction was heated to 80° C. for 12 h. The mixture was concentrated and the crude residue was diluted with EtOAc (75 mL). The organic layer was washed with brine (2×), dried (Na2SO4), and concentrated to an oil. The crude product was purified using radial chromatography (EtOAc:Hex 5:95 to 35:65) to give a colorless oil (0.17 g, 20%). MS (ES) m/e 452 (M+1).

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. additionthe crude residue was diluted with EtOAc (75 mL)
  3. washThe organic layer was washed with brine (2×)
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated to an oil
  6. customThe crude product was purified