HRID484054
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customA thick precipitate was obtained
- filtrationbefore filtering
- customThe solid so obtained
- temperatureheated on the steam bath for 1 hr
- temperaturebefore being cooled
- extractionThis mixture was extracted twice with Et2O
- washthe pooled organic layers were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated to dryness
- customThe residue was crystallized from Et2O-hexane