反応 #79792

ord-15b7fdc006b8414e9f3971f2faa31d6d

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was passed through for 5 minutes
  2. 2
    その他The flask was capped
  3. 3
    その他precipitate formed
  4. 4
    ろ過The solid was collected by filtration

実験手順

3-[4-Amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclopentyl (2S)-2-[(tert-butoxycarbonyl)amino]-3-methylbutanoate (35 mg, 0.060 mmol) was dissolved in ethyl acetate (2.5 ml). Hydrogen chloride gas was passed through for 5 minutes. The flask was capped and the solution stirred for additional 30 minutes. Diethyl ether was added and precipitate formed. The solid was collected by filtration to give 3-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]cyclopentyl (2S)-2-amino-3-methylbutanoate hydrochloride. The structure was confirmed by 1H NMR and LC/MS (MH+=486).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06713474B2uspto-grants-2004_03