反応 #1379893

反応方程式

hydroxylamine

tert-butyldiphenylsilyl chloride

N,N-diisopropylethylamine

N-methyl hydroxylamine hydrochloride

→

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

溶媒

water

dichloromethane

反応条件

後処理

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

実験手順

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).

出典