反应详情

A solution of E2 free base (57.5 mg) in methyl iso-butylketone (0.5 mL) was added to fumaric acid (13.4 mg). Further methyl iso-butylketone (0.5 mL) was added and the mixture was heated with a hot air gun. The resulting yellow gum was scratched with a spatula and a small amount of white solid appeared throughout the gum. The sample was placed on a shaker block and temperature cycled (0-40° C. in 1 h blocks) over the weekend. To the resulting yellow gum in a colourless solution was added 1,4-dioxane (0.5 mL) and the mixture was heated to dissolve the gum. On cooling a gum formed and the sample was temperature cycled as before. After a period of ˜6 weeks a white solid slurry had formed. The mixture was placed back in the shaker block and temperature cycled as before, overnight. The mixture was then left to equilibrate to room temperature and the white solid was collected by filtration. After drying at 40° C. under vacuum overnight the title compound was obtained as a white, mainly crystalline powder (38.7 mg). M.pt. onset ˜150° C.

1. temperaturethe mixture was heated with a hot air gun
2. custom(0-40° C. in 1 h blocks)
3. temperaturethe mixture was heated
4. dissolutionto dissolve the gum
5. temperatureOn cooling a gum
6. customformed
7. customAfter a period of ˜6 weeks a white solid slurry had formed
8. customovernight
9. waitThe mixture was then left
10. customto equilibrate to room temperature
11. filtrationthe white solid was collected by filtration
12. dry with materialAfter drying at 40° C. under vacuum overnight the title compound