تفاعل #462464

ord-d5a49fc567be4958b3b7028bb4ef1fb4

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحIt was filtered through Celite with ethanol and methylene chloride
  2. 2
    أخرىevaporated
  3. 3
    أخرىchromatographed on silica gel using 30% methanol in ethyl acetate as eluant
  4. 4
    أخرىto afford 300 mg (29%) of the less polar diastereomer as an oil and 420 mg (41%) of the more polar diastereomer as an oil

الإجراء التجريبي

A solution of 1.09 g (2.60 mmol) 1-(t-butylacetamido)-3-azido-5,7-diphenylhexahydroazepin-2-one in 30 mL ethanol and 15 mL methylene chloride was hydrogenated at 42 psi in the presence of 0.40 g 10% palladium-on-carbon for 36 hours. The reaction showed Rf 0.30/0.15 iodoplatinate positive, in 30% methanol in ethyl acetate. It was filtered through Celite with ethanol and methylene chloride, evaporated, and chromatographed on silica gel using 30% methanol in ethyl acetate as eluant to afford 300 mg (29%) of the less polar diastereomer as an oil and 420 mg (41%) of the more polar diastereomer as an oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05484917uspto-grants-1996_01