反应 #1095847

ord-03d4c53053494536911020516716c1fe

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩The reaction mixture was concentrated under vacuum, water
  2. 2
    workup.ADDITIONwas added to the residue
  3. 3
    萃取the product was extracted with ethyl acetate
  4. 4
    其他The crude product was purified by conversion into its hydrochloride salt

实验过程

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

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07973020B2uspto-grants-2011_07