反应详情

温度

120 °C

Initially charge 1.0 g (2.97 mmol) of 4-chloro-5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidine and 513 mg (approx. 4.5 mmol) of (+/−)-cis/trans-3-aminocyclohexanol (approx. 3:1 cis/trans mixture; prepared according to J. Chem: Soc. Perkin Trans. I, 1994, 537) in 2.7 ml of DMF. After adding 1.03 ml (5.94 mmol) of DIEA, heat the mixture to 120° C. for 2 h. After cooling, add to ice-water. Filter off the precipitated solid with suction, wash with water and dry under reduced pressure. Purify the crude product by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 2:1→1:2). 1.05 g (85.1% of theory) of the target product are obtained as a cis/trans mixture.

1. temperatureAfter cooling
2. filtrationFilter off the precipitated solid with suction
3. washwash with water
4. customdry under reduced pressure
5. customPurify the crude product by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 2:1→1:2)
6. custom1.05 g (85.1% of theory) of the target product are obtained as a cis/trans mixture