反応 #94591

ord-386fe19412ab46d38012debc49ea6699

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮Then, the reaction mixture was concentrated
  2. 2
    workup.DISSOLUTIONdissolved in 10 ml of water
  3. 3
    その他to give a white gummy precipitate which
  4. 4
    洗浄The chloroform solution was washed with saturated NaCl solution
  5. 5
    乾燥dried over anhydrous sodium sulfate
  6. 6
    その他evaporated in vacuo

実験手順

A solution of 2.4 g of ethyl 1-[N2 -(3-cyclohexyl-4-methoxyphenylsulfonyl)-L-arginyl]-4-methyl-2-piperidinecarboxylate acetate in 10 ml of ethanol and 10 ml of N-NaOH solution was stirred overnight at room temperature. Then, the reaction mixture was concentrated and dissolved in 10 ml of water. The solution was neutralized with 2N-HCl solution to give a white gummy precipitate which was dissolved in 150 ml of chloroform. The chloroform solution was washed with saturated NaCl solution, dried over anhydrous sodium sulfate and evaporated in vacuo to give 1.52 g of 1-[N2 -(3-cyclohexyl-4-methoxyphenylsulfonyl)-L-arginyl]-4-methyl-2-piperidinecarboxylic acid as an amorphous solid. I.R. (KBr): 3350, 2920, 1620, 1250 cm-1.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04131673uspto-grants-1978_12