HRID256572
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 suspension of 2-ethoxycarbonyl-5-bromo-3-chromanone (300 mg, 1 mMol) in methanol (5 mL) and 10% hydrochloric acid (3 mL) was heated at reflux for 2 hours. All of the solid had not dissolved; therefore, trifluoroacetic acid (1 mL) was added, and heating was continued for 18 hours. The reaction mixture was diluted with water and extracted well with diethyl ether. The ether phases were combined, dried over sodium sulfate, and concentrated in vacuo to give a yellow glass. Purification by flash chromatography (1:1 hexane:ether) gave the title compound as a light yellow glass (120 mg, 53%).
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for 2 hours
- dissolutionAll of the solid had not dissolved
- temperatureheating
- extractionextracted well with diethyl ether
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customto give a yellow glass
- customPurification by flash chromatography (1:1 hexane:ether)