HRID1156381

反应详情

EQUATION

反应方程式

HRID 1156381 的结构方程式

CONDITIONS

反应条件

温度
44 °C

PROCEDURE

实验过程

p-Tolyl vinyl sulfone (27.3 g, 0.150 mole) was dissolved in 100 ml of reagent carbon tetrachloride to give a clear solution at 32° C. Addition of 27.3 g (0.172 mole) of m-toluenesulfenyl chloride gave a bright red solution. The exothermic reaction raised the temperature to 44° C. in ten minutes. The color faded to bright orange in 16 hours. Several weeks' standing at room temperature in a closed flask produced crystals. Filtration gave 19.5 g of crude product m.p. 80°-97°. Recrystallization from 50 ml of ethyl acetate-pentane (7:3) gave 13.8 g (27%) of pure product, m.p. 99.5°-100.5°.

WORKUP

后处理

  1. customto give a clear solution at 32° C
  2. customgave a bright red solution
  3. customThe exothermic reaction
  4. custombright orange in 16 hours
  5. customSeveral weeks' standing at room temperature in a closed flask
  6. customproduced crystals
  7. filtrationFiltration
  8. customgave 19.5 g of crude product m.p. 80°-97°
  9. customRecrystallization from 50 ml of ethyl acetate-pentane (7:3)