反应详情

温度

110 °C

A flask was charged with 0.5 g (1.2 mmol) of 2-tert-butyl-5-[2-(2,4-difluoro-benzyl)-butyl]-3-methyl-4-oxo-tetrahydro-pyrimidine-1-carboxylic acid methyl ester, 20 mL dioxane, and 20 mL of conc. HCl solution. The mixture was stirred and heated at 110° C. for 4 days. The solvents were removed under reduced pressure. The residue was taken up in 20 mL of water and 4 drops of conc. HCl solution. The aqueous layer was washed with dichloromethane. The aqueous layer was collected and the water was removed under reduced pressure. The residue was treated with 2 mL of triethylamine, and the excess triethylamine was removed under reduced pressure. The remaining solid was purified by column chromatography (1:8:27 NH4OH, MeOH, dichloromethane eluent). The resulting white solid was washed with acetonitrile and dried under vacuum. This gave 80 mg (24% yield) of the titled compound as a white solid.

1. customThe solvents were removed under reduced pressure
2. washThe aqueous layer was washed with dichloromethane
3. customThe aqueous layer was collected
4. customthe water was removed under reduced pressure
5. additionThe residue was treated with 2 mL of triethylamine
6. customthe excess triethylamine was removed under reduced pressure
7. customThe remaining solid was purified by column chromatography (1:8:27 NH4OH, MeOH, dichloromethane eluent)
8. washThe resulting white solid was washed with acetonitrile
9. customdried under vacuum