تفاعل #1880

ord-42aca8051c1945bf90df0b26f4fe3c47

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  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
    تركيزwhich was then concentrated under reduced pressure The concentrate
  4. 4
    استخلاصwas subjected to extraction with ethyl acetate
  5. 5
    غسيلThe organic layer was washed with water
  6. 6
    أخرىdried
  7. 7
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726306uspto-grants-1998_03