HRID355167

反应详情

EQUATION

反应方程式

HRID 355167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 20.3 g (0.12 mole) of mucochloric acid, 14.1 g (0.12 mole) of indole and 125 ml of benzene was heated for approximately twenty hours at reflux temperature. The reaction mixture was cooled to ambient temperature and a dark brown solid which had separated was collected by filtration. This solid was purified by two successive recrystallizations from benzene at approximately 60° C., with the aid of decolorizing charcoal. After the second recrystallization, the purified product was dried at 60° C. in vacuo to obtain 5.3 g of the known 5-(3-indolyl)-3,4-dichloro-2(5H)-furanone (Formula VI: R=R1 =Y=H), a pale green-colored solid, which first melted at 174° C., then turned black and finally decomposed at 182° C.

WORKUP

后处理

  1. temperaturewas heated for approximately twenty hours
  2. temperatureat reflux temperature
  3. customa dark brown solid which had separated
  4. filtrationwas collected by filtration
  5. customThis solid was purified by two successive recrystallizations from benzene at approximately 60° C., with the aid of decolorizing charcoal
  6. customAfter the second recrystallization
  7. customthe purified product was dried at 60° C. in vacuo