HRID372487

反应详情

EQUATION

反应方程式

HRID 372487 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phenoxathiin-2-carboxylic acid (0.61g) was dissolved in refluxing absolute ethanol (40 ml) and 30% w/v hydrogen peroxide solution (1.50 ml) added. Reflux was maintained for 2 hours, more 30% w/v hydrogen peroxide solution (1.00 ml.) added, and reflux continued for 17 hours. The solution was evaporated to low volume, and the product crystallised out. The solid was filtered, washed and dried to give 2-carboxyphenoxathiin-10-oxide m.p. 223° C. Recrystallisation from absolute ethanol raised the melting point to 237° C.

WORKUP

后处理

  1. additionadded
  2. temperatureReflux
  3. temperaturewas maintained for 2 hours
  4. additionadded
  5. temperaturereflux
  6. customThe solution was evaporated to low volume
  7. customthe product crystallised out
  8. filtrationThe solid was filtered
  9. washwashed
  10. customdried