HRID655156
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
- 0 °C
PROCEDURE
实验过程
Thionyl chloride (10 mL) was added to a solution of 4-hydroxy-4-(3-pyridyl)cyclohexanone ethylene acetal (6.53 g. 27.8 mmol) in pyridine (60 mL) at −10° C. After stirring 0° C. for 30 min, the reaction mixture was poured onto ice. The aqueous layer was adjusted to pH 8 with 2M NaOH aq., and extracted with CH2Cl2, After drying and concentration, the crude product was purified by column chromatography (Hexane/EtOAc=2/1) to yield 4-(3-pyridyl)cyclohex-3-en-1-one ethylene acetal (4.85 g, 62%) as colorless oil.
WORKUP
后处理
- additionthe reaction mixture was poured onto ice
- extractionextracted with CH2Cl2
- customAfter drying
- concentrationconcentration
- customthe crude product was purified by column chromatography (Hexane/EtOAc=2/1)