Reaktion #1882147

ord-86ea44cbb728473f80552b209da791d4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthe reaction mixture was concentrated under reduced pressure
  2. 2
    SonstigeThe residue was purified by column chromatography

Vorschrift

To a solution of (thymin-1-yl)-acetic acid (13 mg, 0.071 mmol), 1-(2-nitro-benzenesulfonyl)-3-phenyl-piperazin-2-one HCl salt (28 mg, 0.070 mmol), and PyBOP (40 mg, 0.077 mmol) in DMF (0.3 mL) was added N,N-diisopropylethylamine (0.018 mL) at room temperature. After stirring for additional 27 h, the reaction mixture was concentrated under reduced pressure. The residue was purified by column chromatography to give the titled compound (16 mg, 43%). 1H NMR (500 MHz; DMSO-d6) δ 11.33 (s, 1H), 8.36 (d, 1H), 8.13 (d, 1H), 8.05˜7.94 (m, 3H), 7.39˜7.29 (m, 5H), 5.93 (s, 1H), 4.87 (d, 1H), 4.67 (d, 1H), 4.22˜4.16 (m, 2H), 3.96 (m, 1H), 3.78 (m, 1H), 1.74 (s, 3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07022851B2uspto-grants-2006_04