反应详情

温度

156 °C

To a solution of N-(4-fluorobenzyl)-3-hydroxy-9-(methylamino)-4-oxo-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidine-2-carboxamide hydrotrifluoroacetate and diisopropylethylamine (4 eqs.) in o-xylene was added Pd(C) (10%). The suspension was stirred and heated to 156° C. for 7 hours. The suspension was left cooling to room temperature and the catalyst was filtered off. The catalyst was washed with methanol and dichloromethane and the filtrate and catalyst washes were combined and the combined organic solutions were concentrated to dryness. The product was purified by preparative RP-HPLC, using water (0.1% TFA) and acetonitrile (0.1% TFA) as eluants (column: C18). After lyophilization of the pooled product fractions the product was obtained as bright yellow fluffy material.

1. waitThe suspension was left
2. temperaturecooling to room temperature
3. filtrationthe catalyst was filtered off
4. washThe catalyst was washed with methanol and dichloromethane
5. concentrationthe combined organic solutions were concentrated to dryness
6. customThe product was purified by preparative RP-HPLC
7. customAfter lyophilization of the pooled product fractions the product was obtained as bright yellow fluffy material