반응 #1379893

반응 방정식

hydroxylamine

tert-butyldiphenylsilyl chloride

N,N-diisopropylethylamine

N-methyl hydroxylamine hydrochloride

→

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

용매

water

dichloromethane

반응 조건

후처리

1. 1
   기타The two layers were separated
2. 2
   추출the aqueous layer was extracted with methylene chloride
3. 3
   건조dried with magnesium sulfate
4. 4
   여과filtered
5. 5
   농축concentrated to dryness under reduced pressure
6. 6
   기타The resulting product was purified by liquid chromatography on silica gel using
7. 7
   workup.ADDITIONa mixture of hexane and ethyl acetate
8. 8
   세척to elute the desired product

실험 절차

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).

출처