تفاعل #5030

ord-caa6c7fdf4b245d7b6e59892ee5ce5b8

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.ADDITIONethyl acetate (500 ml) was added to the residue, which
  4. 4
    غسيلwas then washed with water
  5. 5
    تجفيفdried over anhydrous sodium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off

الإجراء التجريبي

7-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid (6.25 g) was dissolved into DMF (50 ml), to which then potassium carbonate (11 g) and methyl iodide (4.9 ml) were added, and was stirred for 2 hours at room temperature. After the insoluble matter was filtered off and the filtrate was concentrated, ethyl acetate (500 ml) was added to the residue, which was then washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off to give the intended compound 6.65 g (quantitatively) as yellow crystal.

المصدر

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