Reaktion #47042

ord-91bc7a963ab3497ea719c42de6204cea

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 3-methylbenzyl chloride (0.207 mL, 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 180 mg of the product 212. 1H NMR (DMSO-d6) δ 11.21 (s, 2 H), 7.50-7.20 (m, 4 H), 7.20-6.90 (m, 6 H), 6.90-6.65 (m, 4 H), 5.73 (s, 2 H), 4.75 (s, 2 H), 2.32 (s, 3 H); MS: m/z 359 (M++1).

Quelle

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