HRID1439547

反应详情

EQUATION

反应方程式

HRID 1439547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9.1 parts of diethyl 2-methyl-2-[p-(2-naphthoyl)phenyl]malonate, 6 parts of sodium hydroxide and 150 parts of water is stirred and refluxed for 8 hours. The reaction mixture is allowed to stand overnight at room temperature. The whole is diluted with water and the product is extracted with ether. The organic layer is separated and discarded. The aqueous phase is degassed on a rotavapor, filtered and acidified with hydrochloric acid solution; an oil is separated which solidifies on standing. The latter is extracted with ether and the extract is washed with water, dried and evaporated. The residue is crystallized from acetonitrile. The product is filtered off, washed with acetonitrile and dried, yielding p-(2-naphthoyl)hydratropic acid; m.p. 149.7° C.

WORKUP

后处理

  1. temperaturerefluxed for 8 hours
  2. extractionthe product is extracted with ether
  3. customThe organic layer is separated
  4. customThe aqueous phase is degassed on a rotavapor
  5. filtrationfiltered
  6. customan oil is separated which
  7. extractionThe latter is extracted with ether
  8. washthe extract is washed with water
  9. customdried
  10. customevaporated
  11. customThe residue is crystallized from acetonitrile
  12. filtrationThe product is filtered off
  13. washwashed with acetonitrile
  14. customdried