Reaktion #47056

ord-72cd2c4e099f47c8b31ac4d7f85f95f4

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-methylbenzyl chloride (0.204 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 174 mg of the product 227. 1H NMR (DMSO-d6) δ 11.28 (s, 2 H), 7.68 (m, 1 H), 7.55-7.20 (m, 3 H), 7.20-7.00 (m, 6 H), 7.00-6.90 (m, 4 H), 5.82 (s, 2 H), 4.81 (s, 2 H), 2.44 (s, 3 H); MS: m/z 359 (M++1).

Quelle

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