تفاعل #63452

ord-a3652c614646498fbe2e542a6a54e1ec

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONThe reaction mixture is then poured onto ice/water
  2. 2
    استخلاصthe whole is extracted with methylene chloride
  3. 3
    غسيلThe extracts are washed with water
  4. 4
    تجفيفdried over anhydrous sodium sulphate
  5. 5
    أخرىevaporated
  6. 6
    أخرىthe residue is purified by flash chromatography on silica gel [eluent: n-hexane/ethyl acetate (9:1)]

الإجراء التجريبي

A mixture of 1.19 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide (see Example 10), 12 ml of chloroform, 2.7 ml of 50% sodium hydroxide solution and 50 mg of triethylamine is stirred at room temperature for 1 hour. The reaction mixture is then poured onto ice/water and the whole is extracted with methylene chloride. The extracts are washed with water, dried over anhydrous sodium sulphate and evaporated, and the residue is purified by flash chromatography on silica gel [eluent: n-hexane/ethyl acetate (9:1)]. There is obtained 5,7-dihydro-6H-dibenz[c,e]azepine-6-carbonitrile, m.p. 118°-121° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04766115uspto-grants-1988_08