Reaktion #2444253

ord-750539f9ae704bfaa34d9e7287d5f72a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture was filtered through celite and
  2. 2
    Einengenconcentrated

Vorschrift

A solution of benzyl protected acyl-benzohydrazide 5b (1.0 equiv) in MeOH was subjected to hydrogenation in the presence of Pd/C (10% w) for 1 h. The reaction mixture was filtered through celite and concentrated to give compound 5c (6.86 g, 99% yield). MS (ESI, M+Na+): 484.0; TLC (2:1, Hex/EtOAc), Rf=0.20; 1H NMR (400 MHz, CD3OD) δ 8.11 (s, 1H,), 7.95 (d, 1H, J=8.8 Hz), 7.01 (d, 1H, J=8.8 Hz), 4.28 (br s, 1H), 3.91 (br s, 1H), 1.69 (s, 3H,), 1.64 (s, 3H), 1.58 (s, 3H), 1.49 (s, 9H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07759370B2uspto-grants-2010_07