HRID1023932

反应详情

EQUATION

反应方程式

HRID 1023932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-Ethyl-2-(6-fluoro-pyridin-2-yloxy)-phenol (20 mg; 0.09 mmol), under argon, in dimethylformamide (2 mL), cooled to 0° C., was added triethylamine (36 μL; 0.26 mmol) and acetic acid (10 μL; 0.18 mmol). The reaction mixture was allowed to stir overnight, with gradual warming to roomtemperature. The reaction was concentrated, diluted with saturated NaHCO3 (5 mL) and extracted with ethyl acetate (3*3 mL). Combined organic phases were dried over Na2SO4, concentrated in vacuo, the title compound (8 mg; 34%) was obtained as clear oil, after purification on neutral alumina gel (cyclohexane/ethyl acetate: 9/1).

WORKUP

后处理

  1. temperaturewith gradual warming to roomtemperature
  2. concentrationThe reaction was concentrated
  3. additiondiluted with saturated NaHCO3 (5 mL)
  4. extractionextracted with ethyl acetate (3*3 mL)
  5. dry with materialCombined organic phases were dried over Na2SO4
  6. concentrationconcentrated in vacuo