HRID514332

反应详情

EQUATION

反应方程式

HRID 514332 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of phenylacetyl chloride (1 mL, 7.56 mmol) was added dropwise a solution of 2,2-dimethyl-1,3-dioxane-4,6-dione (1.09 g, 7.56 mmol) and pyridine (1.3 mL) in CH2Cl2 (20 mL) at 0° C. The solution was stirred for 30 min at 0° C., then allowed to warm slowly to rt and stirred overnight. The reaction mixture was then washed with 10% aqueous HCl (2×10 mL). The organic layer was dried (MgSO4), filtered, and concentrated under reduced pressure. The crude residue was dissolved in EtOH (20 mL) and heated under reflux conditions for 4 h. The mixture was cooled to rt and then concentrated under reduced pressure. The resulting oil was purified by flash column chromatography (PE/EA=1/4) to afford the title compound (600 mg, 38%) as a yellow oil. [M+H] Calc'd for C12H14O3, 207. Found, 207.

WORKUP

后处理

  1. temperatureto warm slowly to rt
  2. stirringstirred overnight
  3. washThe reaction mixture was then washed with 10% aqueous HCl (2×10 mL)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. dissolutionThe crude residue was dissolved in EtOH (20 mL)
  8. temperatureheated under reflux conditions for 4 h
  9. temperatureThe mixture was cooled to rt
  10. concentrationconcentrated under reduced pressure
  11. customThe resulting oil was purified by flash column chromatography (PE/EA=1/4)