反应详情

219.2 mg (0.76 mmol) 2-Piperidine-4-ylquinoxaline are dissolved in 5.5 mL NMP. After addition of 0.2 mL triethylamine the reaction mixture is stirred for one hour. 200 mg (0.64 mmol) 4-(2-Methyl-6-phenyl-imidazo[1,2-a]pyrimidin-7-yl)benzaldehyde and 0.06 mL acetic acid are added. The reaction mixture is stirred overnight at room temperature. 148 mg (0.7 mmol) NaBH(OAc)3, are added in portions and the reaction mixture is stirred at room temperature for 18 hours. Additionally 75 mg NaBH(OAc)3 and 0.03 mL acetic acid are added and the stirring is continued for four days. The reaction mixture is treated with saturated NaHCO3 and vigorously stirred for one hour. The precipitate is filtered off, washed with water and dried. This solid is treated three times with each 20 mL dichloromethane. After filtration of the combined dichloromethane extracts the filtrate is evaporated and the residue purified by chromatography on silica gel (dichloromethane/methanol). After an additional purification by HPLC 84 mg (25.8%) of the pure product are obtained.

1. stirringThe reaction mixture is stirred overnight at room temperature
2. stirringthe reaction mixture is stirred at room temperature for 18 hours
3. waitthe stirring is continued for four days
4. stirringvigorously stirred for one hour
5. filtrationThe precipitate is filtered off
6. washwashed with water
7. customdried
8. additionThis solid is treated three times with each 20 mL dichloromethane
9. filtrationAfter filtration of the combined dichloromethane
10. customis evaporated
11. customthe residue purified by chromatography on silica gel (dichloromethane/methanol)
12. customAfter an additional purification by HPLC 84 mg (25.8%) of the pure product
13. customare obtained