HRID861990

反应详情

EQUATION

反应方程式

HRID 861990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from Example 26 was dissolved in MEK (180 mL) and placed in a 500 mL flask under a N2 atmosphere. Sodium iodide (catalytic) was added to the reaction which was subsequently stirred at room temperature for 20 min. Triethyl phosphite (3.66 g, 22 mmol) was added to the reaction. The reaction was heated to reflux for 6 h, cooled to room temperature, and stirred an additional 16 h. The reaction was filtered and all solvent removed in vacuo to yield the crude title compound. Purification via flash chromatography (96/4 CHCl3 /EtOH) produced the pure title product.

WORKUP

后处理

  1. customplaced in a 500 mL flask under a N2 atmosphere
  2. temperatureThe reaction was heated
  3. temperatureto reflux for 6 h
  4. temperaturecooled to room temperature
  5. stirringstirred an additional 16 h
  6. filtrationThe reaction was filtered
  7. customall solvent removed in vacuo
  8. customto yield the crude title compound
  9. customPurification via flash chromatography (96/4 CHCl3 /EtOH)