Реакция #1880

ord-42aca8051c1945bf90df0b26f4fe3c47

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONTo the solution was added dropwise
  2. 2
    workup.STIRRINGThe reaction mixture was stirred for one hour at room temperature
  3. 3
    Концентрированиеwhich was then concentrated under reduced pressure The concentrate
  4. 4
    Экстракцияwas subjected to extraction with ethyl acetate
  5. 5
    ПромывкаThe organic layer was washed with water
  6. 6
    Другоеdried
  7. 7
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

Методика

In 20 ml of acetone was dissolved 0.5 g of trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-methanol obtained in Example 46. To the solution was added dropwise, while stirring at room temperature, 0.5 ml of a Jones reagent. The reaction mixture was stirred for one hour at room temperature, which was then concentrated under reduced pressure The concentrate was subjected to extraction with ethyl acetate. The organic layer was washed with water and dried, then the solvent was distilled off under reduced pressure. From the residue was obtained 0.23 g of trans-1-benzyl-7-chloro-5-(2-chlorophenyl)-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-carboxylic acid as white crystals, m.p.177°-178 C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05726306uspto-grants-1998_03