反应详情

温度

50 °C

1-[2-(4-Benzyl-4-hydroxy-piperidin-1-yl)-ethyl]-3-(2-methyl-quinolin-4-yl)-urea (1 equivalent) is dissolved in ethanol at a concentration of 25% w/w and the mixture is heated at 50° C. Aqueous sulfuric acid (1M, 1.1 equivalents) is added. Optionally, the crystallization is initiated by a wet seed of Example 1 (0.5%). The suspension is cooled to 0° C. with a cooling rate of 15° C./h and maintained at this temperature at least 1 hour before filtration and washing with aqueous ethanol (50% W/W). The solid is dried at 30° C. under a wet stream of nitrogen (50% RH) to provide the title compound with a purity of 97.7% with a yield of approximately 90%.

1. customOptionally, the crystallization
2. temperatureThe suspension is cooled to 0° C. with a cooling rate of 15° C./h
3. temperaturemaintained at this temperature at least 1 hour before filtration
4. washwashing with aqueous ethanol (50% W/W)
5. customThe solid is dried at 30° C. under a wet stream of nitrogen (50% RH)