HRID268121
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
To 45 ml. of ethanol was added 8.8 g. of crude ethyl 5-methyl-3-oxo-tetrahydrothiophene-2-carboxylate and 5 g. of 5-(3-methyl-2-octyl) resorcinol. The mixture was cooled in ice and hydrogen chloride was bubbled in for onehalf hour. The mixture was stoppered and let stand at room temperature for 3 days. The reaction mixture was concentrated and dissolved in ether. The ether solution was extracted twice with water and once with aqueous sodium bicarbonate solution. The solution was dried over magnesium sulfate and concentrated. The product was crystallized from acetonitrile to give 4.65 g., m.p. 146°-149°C.
WORKUP
后处理
- temperatureThe mixture was cooled in ice
- customhydrogen chloride was bubbled in for onehalf hour
- concentrationThe reaction mixture was concentrated
- dissolutiondissolved in ether
- extractionThe ether solution was extracted twice with water and once with aqueous sodium bicarbonate solution
- dry with materialThe solution was dried over magnesium sulfate
- concentrationconcentrated
- customThe product was crystallized from acetonitrile
- customto give 4.65 g