反应详情

温度

170 °C

In a 30 ml round-bottomed flask under argon, dissolve 300 mg of [4-(5-methoxycarbonyl-1H-benzimidazol-2-yl)-9H-fluoren-9(R,S)-yl]amide of 1H-pyrrolo[2,3-b]pyridine-4-carboxylic acid, obtained in Example 205, in 5 ml of 3-aminopropanol, and then heat at 170° C. for 2 h 30. The reaction medium is poured into water containing a few ml of ammonia as a 7N solution in sodium chloride methanol, the mixture is extracted with ethyl acetate, and the organic phase is then washed with a saturated solution of sodium chloride, dried over magnesium sulphate and brought to dryness under reduced pressure. The crude solid obtained is purified by flash chromatography on silica gel (40-63 μm), eluting with a mixture of dichloromethane and methanol (95/5 then 9/1 by volume). After formation of a paste with diisopropyl ether, in this way we obtain 38 mg of {{4-{5-[(3-hydroxypropyl)aminocarbonyl]-1H-benzimidazol-2-yl}-9H-fluoren-9(R,S)-yl}}amide of 1H-pyrrolo[2,3-b]pyridine-4-carboxylic acid, in the form of an off-white powder with the following characteristics:

1. extractionthe mixture is extracted with ethyl acetate
2. washthe organic phase is then washed with a saturated solution of sodium chloride
3. dry with materialdried over magnesium sulphate
4. customThe crude solid obtained
5. customis purified by flash chromatography on silica gel (40-63 μm)
6. washeluting with a mixture of dichloromethane and methanol (95/5