Реакция #75390

ord-866b4918b68a46828ad29f644d56bd5a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe mixture was refluxed for 8 hours
  2. 2
    workup.DISTILLATIONthe solvent was distilled off in vacuo
  3. 3
    Экстракцияextracted with chloroform
  4. 4
    ДругоеThe chloroform phase was evaporated
  5. 5
    Другоеthe residue was purified on a silicagel column (eluant: chloroform/acetone 19:1)
  6. 6
    ДругоеThe dihydrochloride was precipitated from acetone/methanol with ethereal hydrochloric acid
  7. 7
    Другоеrecrystallized from acetone/methanol

Методика

4.2 gm of 2,7,7-trimethyl-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione were dissolved in 100 ml of dimethylformamide, and the solution was admixed with 3.4 gm of diethylamino ethyl chloride hydrochloride and 4.1 gm of potassium carbonate. The mixture was refluxed for 8 hours, the solvent was distilled off in vacuo, the residue was admixed with water and extracted with chloroform. The chloroform phase was evaporated and the residue was purified on a silicagel column (eluant: chloroform/acetone 19:1). The dihydrochloride was precipitated from acetone/methanol with ethereal hydrochloric acid and recrystallized from acetone/methanol.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04176184uspto-grants-1979_11