Reaktion #47038

ord-b4f8834e34924bdc90cf458eaecf5cfc

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-chlorobenzyl chloride (0.198 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 105 mg of the product 208. 1H NMR (DMSO-d6) δ 11.38 (s, 2 H), 7.90-7.70 (m, 1 H), 7.70-7.55 (m, 1 H), 7.55-7.35 (m, 2 H), 7.20-7.00 (m, 6 H), 7.00-6.85 (m, 4 H), 5.81 (s, 2 H), 4.88 (s, 2 H); MS: m/z 379 (M++1).

Quelle

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