تفاعل #63452
ord-a3652c614646498fbe2e542a6a54e1ec
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.ADDITIONThe reaction mixture is then poured onto ice/water
- 2استخلاصthe whole is extracted with methylene chloride
- 3غسيلThe extracts are washed with water
- 4تجفيفdried over anhydrous sodium sulphate
- 5أخرىevaporated
- 6أخرىthe 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.