تفاعل #1884

ord-a2fcb8e364ca4dd2ada72db56fde3611

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto be absorbed
  2. 2
    أخرىthe catalyst was removed
  3. 3
    workup.DISTILLATIONby distilling off ethyl acetate under reduced pressure
  4. 4
    أخرىThe residue was crystallized from a small volume of hexane

الإجراء التجريبي

In ethyl acetate (20 ml) was dissolved ethyl ester of trans-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-crotonic acid (0.45 g). To the solution was added 10% palladium carbon (0.1 g), and the mixture was subjected to catalytic reduction at room temperatures under atmospheric pressure. The theoretical amount of hydrogen was allowed to be absorbed, then the catalyst was removed, followed by distilling off ethyl acetate under reduced pressure. The residue was crystallized from a small volume of hexane to give ethyl ester of trans-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-butyric acid (0.37 g) as prisms, m.p.100°-101° C.

المصدر

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