Реакция #83458

ord-3ed4de930d904a0489f463ae423c7990

Растворители

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    КонцентрированиеThe reaction mixture is concentrated in vacuo
  2. 2
    workup.DISSOLUTIONthe residue is dissolved in 100 ml of ethyl acetate
  3. 3
    Промывкаwashed with water, 2N citric acid, aqueous NaHCO3 and brine
  4. 4
    СушкаThe solution is dried with Na2SO4
  5. 5
    Концентрированиеthe volatiles concentrated in vacuo
  6. 6
    Другоеto give a solid which
  7. 7
    Другоеis purified by flash chromatography

Методика

To a mixture of 1.1 mmol of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 10 ml of methylene chloride, cooled to 0° C. is added 1.5 mmol of triethylamine. To the mixture is added 1 mmol of 9,10-dihydro-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine and the mixture stirred at room temperature for 2 hours. The reaction mixture is concentrated in vacuo and the residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, aqueous NaHCO3 and brine. The solution is dried with Na2SO4 and the volatiles concentrated in vacuo to give a solid which is purified by flash chromatography to give the desired product.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05624923uspto-grants-1997_04