HRID1073261

反应详情

EQUATION

反应方程式

HRID 1073261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 12.63 g portion of 2-amino-4'-phenylacetophenone, hydrochloride was dissolved in a mixture of 168 ml of absolute ethanol:water (1:1) and 40 ml of tetrahydrofuran. This solution was kept warm and with stirring, added dropwise to the 5-ethylisatin solution over 2 hours. The mixture was refluxed for 2 hours, then the solvent was distilled off at 85° C. and the reaction cooled for 1 hour. The red solids were collected, stirred with 2 liters of water for 1.5 hours and then filtered. The filtrate was acidified to pH 5 with glacial acetic acid. The resulting yellow solids were collected and dried, giving 4.47 g of the desired product, mp 240°-241° C.

WORKUP

后处理

  1. temperatureThis solution was kept warm
  2. temperatureThe mixture was refluxed for 2 hours
  3. distillationthe solvent was distilled off at 85° C.
  4. temperaturethe reaction cooled for 1 hour
  5. customThe red solids were collected
  6. stirringstirred with 2 liters of water for 1.5 hours
  7. filtrationfiltered
  8. customThe resulting yellow solids were collected
  9. customdried