HRID1084291

反应详情

EQUATION

反应方程式

HRID 1084291 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A stirred mixture of 3 g of 11-(methylsulfonyl)undecanoic acid and 30 mL of methanesulfonic acid was heated to approximately 40° C. The solid dissolved only partially in the methanesulfonic acid at this temperature. Then 1.29 g of 90% hydrogen peroxide was added dropwise. The temperature of the reaction mixture was reduced to room temperature after twenty minutes of reaction time. For the remainder of the two hour reaction time, the reaction mixture was not heated and became homogeneous. The reaction mixture was then cooled in an ice bath forming a solid which was then filtered from solution. The filtrate was poured onto ice prepared from distilled water. A solid formed which was filtered from solution. The two solids collected were combined and washed several times with cold deionized water until the filtrate was no longer strongly acidic. The solid was dried overnight on a watchglass, weighed 2.91 g and had 4.8% by weight active oxygen (84.1% of theoretical).

WORKUP

后处理

  1. customThe temperature of the reaction mixture was reduced to room temperature after twenty minutes of reaction time
  2. customFor the remainder of the two hour reaction time
  3. temperaturethe reaction mixture was not heated
  4. temperatureThe reaction mixture was then cooled in an ice bath
  5. customforming a solid which
  6. filtrationwas then filtered from solution
  7. additionThe filtrate was poured onto ice
  8. customprepared
  9. distillationfrom distilled water
  10. customA solid formed which
  11. filtrationwas filtered from solution
  12. customThe two solids collected
  13. washwashed several times
  14. customThe solid was dried overnight on a watchglass