Реакция #706672

ord-2906667c7b7c40a985e72b8b7df53309

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.DISTILLATIONThe solvent was distilled off
  2. 2
    workup.ADDITIONTo the residue was added chloroform and 2N agueous solution of sodium hydroxide
  3. 3
    ЭкстракцияThe mixture was extracted with chloroform
  4. 4
    СушкаThe extract was dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off

Методика

To a solution of 3.65 g (9.85 mmol) of 1-[1-(tert-butoxycarbonyl)piperidin-4-ylmethyl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one in 30 ml of methanol was added 15 ml of conc. HCl. The mixture was stirred for 1.5 hours at room temperature. The solvent was distilled off. To the residue was added chloroform and 2N agueous solution of sodium hydroxide to make alkaline. The mixture was extracted with chloroform. The extract was dried over anhydrous magnesium sulfate. The solvent was distilled off to give 2.316 g of the desired compound (86.9%, pale yellow solid). This product was used in the subsequent reaction without further purification.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05958942uspto-grants-1999_09