HRID484054

反应详情

EQUATION

反应方程式

HRID 484054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

4'-Hydroxy-2'-methylacetophenone (15 gm, 0.1 mol) was dissolved in pyridine and iodine (25.4 gm) was added. This mixture was heated to 100° C. for 1 hr and then allowed to stand at room temperature overnight. A thick precipitate was obtained and the mixture was diluted with Et2O before filtering. The solid so obtained was added to 5N NaOH (200 ml) and heated on the steam bath for 1 hr before being cooled and acidified with HCl. This mixture was extracted twice with Et2O and the pooled organic layers were washed with brine, dried over Na2SO4, filtered and evaporated to dryness. The residue was crystallized from Et2O-hexane to give 9.8 gm of the title compound as a solid.

WORKUP

后处理

  1. customA thick precipitate was obtained
  2. filtrationbefore filtering
  3. customThe solid so obtained
  4. temperatureheated on the steam bath for 1 hr
  5. temperaturebefore being cooled
  6. extractionThis mixture was extracted twice with Et2O
  7. washthe pooled organic layers were washed with brine
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. customevaporated to dryness
  11. customThe residue was crystallized from Et2O-hexane