Reaktion #983166

ord-8b88031cf02741b48b02275c591a8685

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated
  2. 2
    Sonstigeto give a yellow solid
  3. 3
    Sonstigethat was recrystalized from a mixture of ethanol and diethyl ether

Vorschrift

To a solution of 2-amino-10H-dibenzo[b,f][1,4]oxazepin-11-one (Example 4, 100 mg, 0.44 mmol) in methanol was added thiophene-2-carboximidothioic acid phenyl ester hydrobromide (146 mg, 0.48 mmol). The mixture was stirred at room temperature for 24 hr. The solvent was evaporated to give a yellow solid that was recrystalized from a mixture of ethanol and diethyl ether to give a yellow solid (yield 50 mg, 43%). H1 NMR (DMSO d6) δ: 11.38 (bs, 1H), 10.67 (s, 1H), 9.77 (bs, 1H), 8.95 (bs, 1H), 8.19-8.18 (m, 1H), 8.10 (s, 1H), 7.85 (s, 1H), 7.71-7.68 (m, 1H), 7.55-7.53 (m, 1H), 7.40-7.43 (m, 2H), 7.21-7.18 (m, 3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06919328B1uspto-grants-2005_07