تفاعل #2254213

معادلة التفاعل

2,2-diethyloxan-4-ol

NMO

→

2,2-diethyloxan-4-one

المردود 73.0%

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGto stir for 10 h
2. 2
   ترشيحIt was filtered through a short pad of SiO2
3. 3
   تركيزThe filtrate was concentrated
4. 4
   أخرىpurified by normal phase SiO2 chromatography (0% to 50% EtOAc/hexanes)

الإجراء التجريبي

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%).

المصدر