反应详情

温度

100 °C

0.072 g (0.18 mmol) of methyl 2-amino-6-{[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yl-oxy)phenyl]amino}pyrimidine-4-carboxylate (from example 53) is suspended in 3 ml of water. 0.9 ml of a 1 molar sodium hydroxide solution is added. The reaction mixture is stirred at 100° C. for 18 hours. After cooling, the mixture is adjusted to pH 4.5 using 0.95 ml of a 1N hydrochloric acid solution. The precipitate formed is filtered off with suction and dried. The solid is suspended in DMF. 0.066 mg (0.175 mmol) of HATU, 0.025 g (0.184 mmol) of HOAT, 0.064 ml (0.368 mmol) of diisopropylethylamine and 0.031 g (0.368 mmol) of piperazine are added successively. The reaction mixture is stirred at 40° C. for 5 hours. After cooling, the solution is purified by preparative HPLC. This gives 0.012 g (15% of theory) of product.

1. temperatureAfter cooling
2. customThe precipitate formed
3. filtrationis filtered off with suction
4. customdried
5. stirringThe reaction mixture is stirred at 40° C. for 5 hours
6. temperatureAfter cooling
7. customthe solution is purified by preparative HPLC