Reaktion #47067

ord-9a7e5e914cdb41c6895d132d26387abb

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeevaporated to dryness
  2. 2
    FiltrationThe insoluble material is filtered

Vorschrift

A mixture of intermediate 25 (200 mg, 0.786 mmol) and 2,5-dichlorobenzyl chloride (327 mg, 1.57 mmol) in abs. EtOH (2 mL) is heated at 95° C. for 24 h. The reaction mixture is cooled to RT, evaporated to dryness, and the residue suspended in Et2O. The insoluble material is filtered to give 175 mg of the product 238. 1H NMR (DMSO-d6) δ 11.50 (s, 2 H), 8.00 (s, 1 H), 7.70-7.50 (m, 2 H), 7.20-7.00 (m, 6 H), 6.95-6.80 (m, 4 H), 5.81 (s, 2 H), 4.90 (s, 2 H); MS: m/z 413 (M++1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741493B2uspto-grants-2010_06