Method for the purification of Piribedil
View Patent ↗A method for purifying Piribedil includes mixing Piribedil solid having a purity of 98% by weight with water, boiling the mixture, adding slowly 95% ethanol to the boiling mixture to form a clear liquid, filtering the hot clear liquid, cooling the filtrate to obtain a white crystal having a purity of 99.8% by weight of Piribedil.
1. A method for purifying Piribedil comprising the following steps: a) mixing a Piribedil product having a Piribedil purity of 98 wt % or lower with water; b) heating the resulting mixture to boiling or a temperature near boiling; c) adding ethanol to the hot mixture from step b) while maintaining a temperature of the resulting mixture at 60–100° C., so that a clear liquid is obtained; d) filtering the hot clear liquid; e) cooling the resulting filtrate to form a crystal therein; and f) removing the crystal from the filtrate and drying the crystal to obtain a white solid having a Piribedil purity higher than 98 wt %.
2. The method according to claim 1 , wherein the Piribedil product having a Piribedil purity of 98 wt % or lower used in step a) has a Piribedil purity of about 98 wt %.
3. The method according to claim 1 , wherein in step a) the Piribedil product having a Piribedil purity of 98 wt % or lower is mixed with water in a ratio of per kilogram of the Piribedil product 0.1–10 liters of water.
4. The method according to claim 3 , wherein in step a) the Piribedil product having a Piribedil purity of 98 wt % or lower is mixed with water in a ratio of per kilogram of the Piribedil product about one liter of water.
5. The method according to claim 2 , wherein in step a) the Piribedil product having a Piribedil purity of 98 wt % is prepared from a method comprising reacting 1-(2-pyrimidinyl)piperazine and piperonal in the presence of formic acid as a reducing agent at a temperature of 100–140° C.
6. The method according to claim 1 , wherein the ethanol used in step c) is an aqueous solution having an ethanol concentration of 25–95 wt %.
7. The method according to claim 1 , wherein the ethanol used in step c) is an aqueous solution having an ethanol concentration of 95 wt %.
8. The method according to claim 7 , wherein in step c) the ethanol added is in an amount of 1–100 liters per kilogram of the Piribedil product.
9. The method according to claim 8 , wherein in step c) the ethanol added is in an amount of 10 liters per kilogram of the Piribedil product.
10. The method according to claim 1 , wherein the white solid obtained in step f) has a Piribedil purity of 99.8 wt %.