تفاعل #1379324

ord-3d027f9c432344bc8281a9239dc782a0

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was removed under vacuum
  2. 2
    أخرىformed
  3. 3
    أخرىThe solid was collected
  4. 4
    أخرىrecrystallised from methanol-water

الإجراء التجريبي

To a solution of 2-amino-3-methylbenzamide (0.5 g, 3.3 mmol) (prepared by conventional methods) and pyridine (0.35 ml, 4.3 mmol) in dry THF (15 ml), was added a solution of acetyl chloride (0.36 ml, 5.0 mmol) in THF (2 ml) dropwise, and the mixture was stirred overnight under nitrogen. The solvent was removed under vacuum and the remaining white slurry was resuspended in 2% aqueous sodium hydroxide solution and neutralised with aqueous hydrochloric acid, whereupon a white precipitate formed. The solid was collected and recrystallised from methanol-water to furnish the required quinazolinone (0.47 g, 81%) m.p. 217°-220° C.;

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05756510uspto-grants-1998_05