HRID2291906

反应详情

EQUATION

反应方程式

HRID 2291906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Acetyl-3a,7a-dihydro-7a-(phenylethynyl)benzofuran-2,5(3H,4H)dione, (1.75 g 6 mmole), pyridinium chloride (1.5 g, 13 mmole) and MeOH (50 mL) were placed in a 100 mL round bottomed flask and heated at reflux for 2 hr. The solvent was removed under reduced pressure and the residue was partitioned between Et2O and water. The ether phase was washed with 3N hydrochloric acid, dried over anhydrous sodium sulfate, filtered and concentrated. The residue was recrystallized from ethanol (10 mL) to give 0.8 g (50%) of the title compound as a light yellow solid, m.p. 63°-65° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 2 hr
  3. customThe solvent was removed under reduced pressure
  4. customthe residue was partitioned between Et2O and water
  5. washThe ether phase was washed with 3N hydrochloric acid
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was recrystallized from ethanol (10 mL)