HRID1586373

反应详情

EQUATION

反应方程式

HRID 1586373 的结构方程式

PROCEDURE

实验过程

Initially, α-bromolauric acid methyl ester was prepared as follows. Pure lauric acid (100 gm 0.5 mol) was dissolved in thionyl chloride (89 gm, 0.75 mol) at 55° C. under nitrogen. A large amount of hydrogen chloride gas was generated. When all the lauric acid was converted to acid chloride and there was no more HCl gas being generated after stirring for 2.5 hours, bromine (89.25 gm, 0.65 mol) was slowly added to the solution at room temperature. The reaction mixture was stirred for another 8 hours at 45° C. The reaction was then stopped by evaporating additional bromine at 80° C. by bubbling in nitrogen. The crude product, α-bromolauric acid chloride, was cooled to 0° under nitrogen. Pure methanol was then added very slowly to the acid chloride solution at 0° C. The temperature was not allowed to exceed 15° C. during this process. The final crude product, α-bromolauric acid methyl ester, was washed with water several times. The final product was extracted twice with hexane. The NMR results showed that the product was completely pure. The yield of the reaction was about 98% and may be summarized as follows: ##STR7## B. Preparation of Hydroquinone Bislauric Acid Methyl Ester (2)

WORKUP

后处理

  1. stirringThe reaction mixture was stirred for another 8 hours at 45° C
  2. customby evaporating additional bromine at 80° C.
  3. customby bubbling in nitrogen
  4. temperatureThe crude product, α-bromolauric acid chloride, was cooled to 0° under nitrogen
  5. additionPure methanol was then added very slowly to the acid chloride solution at 0° C
  6. customto exceed 15° C. during this process
  7. washThe final crude product, α-bromolauric acid methyl ester, was washed with water several times
  8. extractionThe final product was extracted twice with hexane
  9. customThe NMR results