反应详情

温度

150 °C

A mixture of 2-[4-[chloro(4-chlorophenyl)methyl]-3,5-dichlorophenyl]-1,2,4-triazine-3,5(2H,4H)-dione (0.00719 mol) and 2-pyrimidinamine (0.00863 mol) was heated for 2 hours at 150° C. in an autoclave. The mixture was cooled to RT. This fraction was taken up into CH2Cl2, washed with water, dried, filtered and the solvent was evaporated. The residue was purified by HPLC (eluent: (0.5% NH4OAc in H2O)/CH3OH/CH3CN gradient elution from 70/15/15 over 0/50/50 to 0/0/100). The desired fractions were collected and the solvent was evaporated. The residue was coevaporated with EtOAc. The residue was stirred in DIPE, filtered off, washed and dried, yielding 0.21 g of (±)-2-[3,5-dichloro-4-[(4-chlorophenyl)[(2-pyrimidinyl)amino]-methyl]phenyl]-1,2,4-triazine-3,5(2H,4H)-dione (comp. 413).

1. temperatureThe mixture was cooled to RT
2. washwashed with water
3. customdried
4. filtrationfiltered
5. customthe solvent was evaporated
6. customThe residue was purified by HPLC (eluent: (0.5% NH4OAc in H2O)/CH3OH/CH3CN gradient elution from 70/15/15 over 0/50/50 to 0/0/100)
7. customThe desired fractions were collected
8. customthe solvent was evaporated
9. filtrationfiltered off
10. washwashed
11. customdried