反応 #1269839

ord-91cccc8fe93f40d99bcf8c3ba833bdba

反応方程式

CCOC(=O)CCN(CC(=O)OCC)C(=O)CCCCCNC(=O)OCC1c2ccccc2-c2ccccc21
3-{Ethoxycarbonylmethyl-[6-(9H-fluoren-9-ylmethoxycarbonylamino)-hexanoyl]-amino}-propionic acid ethyl ester
CCOC(=O)CCN(CC(=O)OCC)C(=O)CCCCCN
3-[(6-Amino-hexanoyl)-ethoxycarbonylmethyl-amino]-propionic acid ethyl ester

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction mixture is concentrated under vacuum, water
  2. 2
    workup.ADDITIONis added to the residue
  3. 3
    抽出the product is extracted with ethyl acetate
  4. 4
    その他The crude product is purified by conversion into its hydrochloride salt

実験手順

3-{Ethoxycarbonylmethyl-[6-(9H-fluoren-9-ylmethoxycarbonylamino)-hexanoyl]-amino}-propionic acid ethyl ester AB (11.5 g, 21.3 mmol) is dissolved in 20% piperidine in dimethylformamide at 0° C. The solution is continued stifling for 1 h. The reaction mixture is concentrated under vacuum, water is added to the residue, and the product is extracted with ethyl acetate. The crude product is purified by conversion into its hydrochloride salt.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08664193B2uspto-grants-2014_03