HRID655156

反应详情

EQUATION

反应方程式

HRID 655156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionthe reaction mixture was poured onto ice
  2. extractionextracted with CH2Cl2
  3. customAfter drying
  4. concentrationconcentration
  5. customthe crude product was purified by column chromatography (Hexane/EtOAc=2/1)