HRID2198616

反应详情

EQUATION

反应方程式

HRID 2198616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 1.19 g. portion of the product of Example 30 above, 20 ml. of anhydrous dimethylformamide and 3.4 g. of freshly distilled pyrrolidine were added to a flask at 25°, and then 100 mg. of powdered potassium iodide was added and the mixture was stirred at ambient temperature for 1 hour. The mixture was then evaporated under vacuum, 25 ml. of saturated aqueous sodium bicarbonate was added, and the mixture was extracted twice with 25 ml. portions of ethyl acetate. The extract was washed five times with 20 ml. portions of aqueous sodium chloride, and was dried over magnesium sulfate and evaporated to a brown oil. The oil was dissolved in 25 ml. of hydrochloric acid in methanol, which had been prepared by addition of 10 ml. of acetyl chloride to 100 ml. of methanol under nitrogen at 0°. The mixture was then evaporated to dryness under vacuum, and the resulting foam was crystallized from denatured ethanol to provide 1.07 g. of crystals, m.p. 206°-207°.

WORKUP

后处理

  1. customThe mixture was then evaporated under vacuum, 25 ml
  2. additionof saturated aqueous sodium bicarbonate was added
  3. extractionthe mixture was extracted twice with 25 ml
  4. washThe extract was washed five times with 20 ml
  5. dry with materialportions of aqueous sodium chloride, and was dried over magnesium sulfate
  6. customevaporated to a brown oil
  7. dissolutionThe oil was dissolved in 25 ml
  8. customof hydrochloric acid in methanol, which had been prepared by addition of 10 ml
  9. customat 0°
  10. customThe mixture was then evaporated to dryness under vacuum
  11. customthe resulting foam was crystallized from denatured ethanol
  12. customto provide 1.07 g