HRID372940

反应详情

EQUATION

反应方程式

HRID 372940 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 11.26 grams (0.05 mol) of sodium m-nitrobenzenesulfonate in 50 milliters of water was added to a solution of 15.94 grams (0.05 mol) of the N,N-dimethyl-N-(2-benzoylaminoethyl)benzylammonium chloride, prepared as described in Example 2, in 50 milliters of water. An oily precipitate formed. The water layer was decanted and the oil was rinsed with water, dissolved in methylene chloride, dried over magnesium sulfate and concentrated to a viscous oil. The oil was treated with ligroine (bp=35°-60° C.) with warming. The oil crystallized and the solid formed was collected and recrystallized from isopropanol. The yield of product was 10.75 grams (44.28% of theory); mp=109°-112° C.

WORKUP

后处理

  1. customprepared
  2. customAn oily precipitate formed
  3. customThe water layer was decanted
  4. washthe oil was rinsed with water
  5. dissolutiondissolved in methylene chloride
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated to a viscous oil
  8. additionThe oil was treated with ligroine (bp=35°-60° C.)
  9. temperaturewith warming
  10. customThe oil crystallized
  11. customthe solid formed
  12. customwas collected
  13. customrecrystallized from isopropanol