Reaktion #157050

ord-15eb03f88afe4dd7b5b57a57fa19cdb4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwas washed with H2O, Na2CO3(sat), NaCl(sat.)
  2. 2
    Trocknenwas dried over MgSO4
  3. 3
    Filtrationwas filtered
  4. 4
    Sonstigethe volatiles were removed in vacuo

Vorschrift

A solution containing 1.0 eq each of 1-(3-nitropyridin-4-yl)piperazine, N-Boc-beta-alanine, HOAT and EDC in DCM, at a concentration of 0.1 M, was stirred for 16 hours. The solution was diluted with EtOAc and was washed with H2O, Na2CO3(sat), NaCl(sat.), was dried over MgSO4, was filtered and the volatiles were removed in vacuo yielding tert-butyl 3-(4-(3-nitropyridin-4-yl)piperazin-1-yl)-3-oxopropylcarbamate (93%). LCMS (m/z): 379.9 (MH+); LC Rt=1.92 min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822497B2uspto-grants-2014_09