HRID1863146

反应详情

EQUATION

反应方程式

HRID 1863146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

40.0 G. (0.25 mole) of 3-methylnonan-3-ol, 20. g. of pyridine and 60 ml. of toluene are combined and cooled to 5° C. under agitation. To the resulting solutin is added, under agitation, over a period of 1 to 2 hours while maintaining the reaction temperature between 5°-15° C., a solution of 35.15 g. (0.25 mole) of benzoyl chloride, dissolved in 30 ml. of toluene. The source of cooling is removed and the reaction mixture is agitated overnight, permitting the temperature of the reaction mixture to rise to room temperature (25°-30° C.). After completion of the reaction, the formed pyridine hydrochloride is removed by successive washings with 100 ml. of warm water. The solvent is removed by distillation and the desired ester is rectified by fractional distillation in a vacuum, preferably at 1 mm.

WORKUP

后处理

  1. additionTo the resulting solutin is added, under agitation, over a period of 1 to 2 hours
  2. temperaturewhile maintaining the reaction temperature between 5°-15° C.
  3. temperatureThe source of cooling
  4. customis removed
  5. customto rise to room temperature
  6. custom(25°-30° C.)
  7. customAfter completion of the reaction
  8. customthe formed pyridine hydrochloride is removed by successive washings with 100 ml
  9. customThe solvent is removed by distillation
  10. distillationthe desired ester is rectified by fractional distillation in a vacuum, preferably at 1 mm