反応 #1379892

ord-423113c6f9214254b81f248800c52937

反応方程式

CC(C)(C)OC(=O)NCC(NC(=O)OC(C)(C)C)C(=O)OCc1ccccc1
2,3-bis-tert-butoxycarbonylamino propionic acid benzyl ester
Cl
HCl
Cl.Cl.Cl.NCC(N)C(=O)O
2,3-Diamino-propionic acid trihydrochloride

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was removed under vacuum
  2. 2
    workup.ADDITIONthe mixture was diluted with ethyl acetate (100 ml) and water (50 ml)
  3. 3
    その他The layers were separated
  4. 4
    その他the aqueous layer was evaporated to dryness (1.23 g of a foam/syrup)

実験手順

A solution of 2,3-bis-tert-butoxycarbonylamino propionic acid benzyl ester (1.8 g), 4N aqueous HCl (40 ml), and acetonitrile (50 ml) was stirred for 18 hours at room temperature. The solvent was removed under vacuum, and the mixture was diluted with ethyl acetate (100 ml) and water (50 ml) and stirred for 15 minutes. The layers were separated and the aqueous layer was evaporated to dryness (1.23 g of a foam/syrup). 1H NMR (300 MHz): 3.2-3.5 (m, 2H), 4.2-4.35 (m, 1H), 5.13-5.25 (q, 2H, J=11.8, 3.1 Hz).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07238341B2uspto-grants-2007_07