反应详情

温度

55 °C

Alternatively, 1.0 g of 2-chloro-4-(4-nitrophenyloxy)-5-trifluoromethylpyrimidine is dissolved in 5 mL of 1-methyl-2-pyrrolidinone (NMP). 1.44 g of the mono-4-toluenesulfonic acid salt of 4-amino-N-methyl-N-(1-methyl-piperidin-4-yl)-benzamide, 76 μL of trimethylsilylchloride (as water scavenger) and 60 mg methanesulfonic acid are added. The suspension is stirred for 18 hours at 55° C. 15 mL methylenechloride and 10 mL 2N sodium hydroxide solution are added. The organic phase is separated and the solvent is reduced so that 5 g of a concentrated solution remain. To this solution 20 mL 2-propanol and 0.32 g methanesulfonic acid are added. Crystallization occurs. The suspension is filtered, washed and dried to obtain 1.5 g (77% of theory) of product N-methyl-N-(1-methyl-piperidin-4-yl)-4-[4-(4-nitro-phenoxy)-5-trifluoromethyl-pyrimidin-2-ylamino]-benzamide as methanesulfonic acid salt.

1. customThe organic phase is separated
2. additionTo this solution 20 mL 2-propanol and 0.32 g methanesulfonic acid are added
3. customCrystallization
4. filtrationThe suspension is filtered
5. washwashed
6. customdried