HRID1902756
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
PROCEDURE
实验过程
A solution of 1.3 g of ethyl 2-[4-(2-oxo-1-cyclohexylidenemethyl)phenyl]propionate in 15 ml of dioxane and 100 ml of a 10% aqueous solution of hydrogen bromide was heated under reflux for 1 hour. After cooling, the reaction mixture was extracted with ether. The extract was washed with water and dried over anhydrous sodium sulfate. The ether was distilled off to leave an oily substance, which was then vacuum distilled to give 0.6 g of the desired product having a boiling point of 210°-215° C./0.3 mmHg (bath temp.). This product solidified and crystallized after cooling. m.p. 108°-110° C.
WORKUP
后处理
- temperatureunder reflux for 1 hour
- temperatureAfter cooling
- extractionthe reaction mixture was extracted with ether
- washThe extract was washed with water
- dry with materialdried over anhydrous sodium sulfate
- distillationThe ether was distilled off
- customto leave an oily substance, which
- distillationvacuum distilled