HRID76225

反应详情

EQUATION

反应方程式

HRID 76225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of crude 2,2-diethyloxan-4-ol (500 mg, 3.2 mmol) in CH2Cl2 (10 ml) were added NMO (750 mg, 6.41 mmol) and 4 A molecular sieves (2 g). The solution was stirred for 30 mins and then TPAP (34 mg, 0.096 mmol) was added in one portion. The reaction was allowed to stir for 10 h. After checking the TLC, the alcohol was gone. It was filtered through a short pad of SiO2. The filtrate was concentrated and purified by normal phase SiO2 chromatography (0% to 50% EtOAc/hexanes) to give 2,2-diethyloxan-4-one (365 mg, 73%).

WORKUP

后处理

  1. stirringto stir for 10 h
  2. filtrationIt was filtered through a short pad of SiO2
  3. concentrationThe filtrate was concentrated
  4. custompurified by normal phase SiO2 chromatography (0% to 50% EtOAc/hexanes)