反应详情

Acetone (7 ml) was added to tartaric acid (126.15 mg, 1 eg) in order to dissolve the acid. The acid solution was then added to 500 mg of (5R)-5-[5-[{2-[3,5-bis(trifluoromethyl)phenyl]-2-methylpropanoyl}(methyl)amino]-4-(4-fluoro-2-methylphenyl)-2-pyridinyl]-2-methyl-D-prolinamide (Example 1). The resulting slurry was set up to temperature cycle (0-40° C.) whilst stirring at 500 rpm. After 1 hour, a thick, gel-like material had formed. Further acetone (13 ml) was then added in order to improve the mobility of the material. The reaction was temperature cycled for a further 3 days whilst stirring. The solid was then isolated and allowed to dry at 45° C. overnight to obtained the title compound in a crystalline form (463 mg). Onset melt 211° C. by DSC.

1. dissolutionto dissolve the acid
2. customwas set up to temperature cycle (0-40° C.)
3. customa thick, gel-like material had formed
4. waitcycled for a further 3 days
5. stirringwhilst stirring
6. customThe solid was then isolated
7. customto dry at 45° C. overnight