تفاعل #1379893

معادلة التفاعل

hydroxylamine

tert-butyldiphenylsilyl chloride

N,N-diisopropylethylamine

N-methyl hydroxylamine hydrochloride

→

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

المذيبات

water

dichloromethane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر