反应详情

To a solution of 2,4,6-trichloro-5-nitro pyrimidine (Intermediate 37, 1 g, 4.4 mmol) in EtOH at −50° C. were added 5-methyl-1H-pyrazol-3-amine (255 mg) and DIPEA (1.6 ml) drop-wise. The resulting mixture was stirred at this temperature for 5 minutes whereupon 4-amino pyran (300 mg) was added. The resulting mixture was allowed to warm to ambient temperature for 4 hours. The mixture was diluted with H2O and EtOAc and the aqueous layer was extracted with EtOAc. The combined organic layers were washed with brine, saturated NaHCO3 (aq) solution, dried and evaporation of the volatiles under reduced pressure gave a colored residue. Purification by Gilson (MeCN/H2O, 5%→95%, 15 minutes) gave the title compound (120 mg). LCMS: 354 [M+1].

1. additionwas added
2. extractionthe aqueous layer was extracted with EtOAc
3. washThe combined organic layers were washed with brine, saturated NaHCO3 (aq) solution
4. customdried
5. customevaporation of the volatiles under reduced pressure
6. customgave a colored residue
7. customPurification by Gilson (MeCN/H2O, 5%→95%, 15 minutes)