Реакция #3647

ord-b2aca09294cd4507a7fd38eab4bba6a8

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ПромывкаThe reaction mixture is washed with water, 2N citric acid, NaHCO3, and brine
  2. 2
    СушкаThe reaction mixture is dried with Na2SO4
  3. 3
    Фильтрацияfiltered
  4. 4
    Другоеevaporated in vacuo
  5. 5
    Другоеto give a solid which
  6. 6
    Другоеis purified by flash chromatography on silica gel

Методика

To a stirred solution of 3 mmol of 2-methylbenzoyl chloride in 10 ml of methylene chloride is added 5 mmol of triethylamine and 3 mmol of 4,10-dihydro-4-(4-aminobenzoyl)-5H-pyrrolo-[1,2-a]thieno[3,2-e][1,4]diazepine. The mixture is stirred for 5 hours. The reaction mixture is washed with water, 2N citric acid, NaHCO3, and brine. The reaction mixture is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography on silica gel to give the desired product as a solid, m.p. 162°-188° C. (amorphous)

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05733905uspto-grants-1998_03