تفاعل #1964647

ord-2e5969c61461401c8510aac5b16cb34a

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىobtained
  2. 2
    أخرىAfter treatment as in stage 3 of Example 3, and then purification by flash chromatography
  3. 3
    غسيلon silica gel, elution
  4. 4
    أخرىfollowed by crystallization from 10 ml of diisopropyl ether, 200 mg of 2-(2-carbamoylethylamino)-4-[4-(6-fluoro-1H-benzimidazol-2-yl)-9H-carbazol-9-yl]benzamide
  5. 5
    أخرىare thus obtained in the form of a beige solid

الإجراء التجريبي

The process is carried out as in stage 3 of Example 3, but using 300 mg of 2-fluoro-4-[4-(6-fluoro-1H-benzimidazol-2-yl)carbazol-9-yl]benzonitrile, obtained according to stage 2 of Example 3, 296 mg of potassium carbonate, 1.779 g of beta-alanineamide hydrochloride and 1.445 g of triethylamine in 3 ml of dimethyl sulphoxide. 1.357 ml of a 1M aqueous solution of sodium hydroxide, 1.313 ml of a 30% aqueous solution of hydrogen peroxide and 7 ml of ethanol are then added to the reaction medium. After treatment as in stage 3 of Example 3, and then purification by flash chromatography on silica gel, elution being carried out with mixtures of dichloromethane and ethanol (from 95/5 to 90/10 by volume), followed by crystallization from 10 ml of diisopropyl ether, 200 mg of 2-(2-carbamoylethylamino)-4-[4-(6-fluoro-1H-benzimidazol-2-yl)-9H-carbazol-9-yl]benzamide are thus obtained in the form of a beige solid, the characteristics of which are the following:

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08309721B2uspto-grants-2012_11