تفاعل #5028

ord-53267f682d9a4174af11e039aaa24acc

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحAfter the insoluble matter was filtered off
  2. 2
    تركيزthe filtrate was concentrated
  3. 3
    workup.ADDITIONa mixed liquid of ethyl acetate-benzene (1:1, 400 ml) was added to the residue
  4. 4
    غسيلthe mixture was washed with water
  5. 5
    تجفيفdried over anhydrous sodium sulfate
  6. 6
    workup.DISTILLATIONto distilling off the solvent

الإجراء التجريبي

To 7-bromo-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid (8.53 g) dissolved in DMF (80 ml), were added potassium carbonate (13.8 g) and benzyl bromide (4.5 ml) and the mixture was stirred for 2 hours at room temperature. After the insoluble matter was filtered off and the filtrate was concentrated, a mixed liquid of ethyl acetate-benzene (1:1, 400 ml) was added to the residue, and the mixture was washed with water, dried over anhydrous sodium sulfate and then subjected to distilling off the solvent to give the intended compound 11.35 g (99.7%) as brown oily matter.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05242912uspto-grants-1993_09