反応 #1904052

ord-53d880317f8844c4886300d5a5deb433

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The methylene chloride solution is subsequently washed successively with 10 ml of each of 1N hydrochloric acid, saturated sodium hydrogencarbonate solution and water
  2. 2
    乾燥dried over sodium sulfate
  3. 3
    workup.ADDITION10 ml of diethyl ether are added to the residue
  4. 4
    ろ過the white precipitate deposited is filtered off

実験手順

5.4 The solution of 0.2 g (0.54 mmol) of dimethyl (S)-{2-amino-2-[4-(3-oxomorpholin-4-yl)phenylcarbamoyl]ethyl}phosphonate and 0.092 g (0.54 mmol) of 4-chlorophenyl isocyanate in 10 ml of dichloromethane is stirred at room temperature for 12 hours. The methylene chloride solution is subsequently washed successively with 10 ml of each of 1N hydrochloric acid, saturated sodium hydrogencarbonate solution and water and dried over sodium sulfate. After the solvent has been stripped off, 10 ml of diethyl ether are added to the residue, and the white precipitate deposited is filtered off, giving 0.28 g (100%) of (S)-2-[3-(4-chlorophenyl)ureido]-N-[4-(3-oxomorpholin-4-yl)phenyl]-3-(dimethoxyphosphoryl)propionamide (“1D”), ESI 525.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07598241B2uspto-grants-2009_10