반응 #1964673

ord-72b33dfe66d8496db9b2f30576424085

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타obtained
  2. 2
    기타After treatment as in stage 3 of Example 3, and then purification by flash chromatography
  3. 3
    세척on silica gel, elution
  4. 4
    workup.ADDITIONbeing carried out with a mixture of dichloromethane and ethanol (95/5 by volume), 35 mg of 414-(6-fluoro-1H-benzimidazol-2-yl)-9H-carbazol-9-yl]-2-[(pyridin-3-ylmethyl)-amino]benzamide
  5. 5
    기타are thus obtained in the form of a white powder

실험 절차

The process is carried out as in stage 3 of Example 3, but using 168.2 mg of 2-fluoro-4-[4-(6-fluoro-1H-benzimidazol-2-yl)-9H-carbazol-9-yl]benzonitrile, obtained according to stage 2 of Example 3, 166 mg of potassium carbonate and 346 mg of 3-(aminomethyl)pyridine in 1.7 ml of dimethyl sulphoxide, in a microwave for 1 hour and 30 minutes at 115° C. 0.76 ml of a 1M aqueous solution of sodium hydroxide, 0.735 ml of a 30% aqueous solution of hydrogen peroxide and 4 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 a mixture of dichloromethane and ethanol (95/5 by volume), 35 mg of 414-(6-fluoro-1H-benzimidazol-2-yl)-9H-carbazol-9-yl]-2-[(pyridin-3-ylmethyl)-amino]benzamide are thus obtained in the form of a white powder, the characteristics of which are the following:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08309721B2uspto-grants-2012_11