反应 #1379893

反应方程式

hydroxylamine

tert-butyldiphenylsilyl chloride

N,N-diisopropylethylamine

N-methyl hydroxylamine hydrochloride

→

N-Methyl,N-(tert-butyldiphenylsilyl)hydroxylamine

溶剂

water

dichloromethane

反应条件

后处理

1. 1
   其他The two layers were separated
2. 2
   萃取the aqueous layer was extracted with methylene chloride
3. 3
   干燥dried with magnesium sulfate
4. 4
   过滤filtered
5. 5
   浓缩concentrated to dryness under reduced pressure
6. 6
   其他The resulting product was purified by liquid chromatography on silica gel using
7. 7
   workup.ADDITIONa mixture of hexane and ethyl acetate
8. 8
   洗涤to elute the desired product

实验过程

One possible synthetic scheme for hydroxylamine derivatives involves adding tert-butyldiphenylsilyl chloride and N,N-diisopropylethylamine to a suspension of N-methyl hydroxylamine hydrochloride in dry dichloromethane. The reaction mixture was stirred followed by the addition of water. The two layers were separated and the aqueous layer was extracted with methylene chloride. The organic solutions were then combined, dried with magnesium sulfate, filtered, and concentrated to dryness under reduced pressure. The resulting product was purified by liquid chromatography on silica gel using a mixture of hexane and ethyl acetate to elute the desired product. The purification process gave N-Methyl,N-(tert-butyldiphenylsilyl)hydroxylamine (27).

来源