Patent ID: 8569492

Claim:
A method for preparing halofuginone compounds comprising the following steps: (1) reacting a condensate of formula (II) for 12-35 hours in a catalytic hydrogenation solvent under 10˜60° C. and 0.1˜1.0 MPa controlled hydrogen pressure, with presence of a Ni—B non-crystalline alloy catalyst, as shown in the following reaction formula: wherein the Ni—B non-crystalline alloy catalyst is prepared by loading a Ni—B non-crystalline alloy on an aluminium oxide or zeolite carrier, with a load of 1.0˜20.0% as a weight percentage; wherein the weight ratio between the Ni—B non-crystalline alloy catalyst and the condensate (II) is 1:10˜40; wherein the catalytic hydrogenation solvent is a 0.1˜0.6N acidic aqueous alcohol solution containing a mass of the catalytic hydrogenation solvent being 8-20 times that of the condensate (II); wherein the Ni—B non-crystalline alloy catalyst is prepared as follows: adding a nickel salt into an aqueous solvent until the salt is dissolved; then adding a carrier selected from the group consisting of aluminium oxide and zeolite; adding a KBH4 solution drip by drip under 0˜30° C.; after above reaction is over, filtering the solution, washing precipitates with deionized water until pH reaches 6.5˜7.5, and finally storing treated precipitates in anhydrous ethanol for use; the nickel salt above is Ni(NO 3 ) 2 , NiCl 2 or Ni(SO 4 ); (2) filtering the Ni—B non-crystalline alloy catalyst and treating yielded filtrate to obtain crude 3-[3-[(2R,3S)-3-hydroxyl-2-piperidinyl]-2-oxypropyl]-4(3H)-quinazolinone compounds (I); (3) through refining procedures, obtaining refined 3-[3-[(2R,3S)-3-hydroxyl-2-piperidinyl]-2-oxypropyl]-4(3H)-quinazolinone compounds (I); wherein the refining procedures are as follows: adding the crude 3-[3-[(2R,3S)-3-hydroxyl-2-piperidinyl]-2-oxypropyl]-4(3H)-quinazolinone compounds to a re-crystallizing solvent for reflux for more than 8 hours, then decolorizing it with activated carbon and crystallizing it under 0˜40° C. for 3-8 hours to obtain refined product; wherein the re-crystallizing solvent is a mixed solution of alcohol, water and halohydrocarbon, the amount of the mixed solution is 5-15 times of the amount of the crude 3-[3-[(2R,3S)-3-hydroxyl-2-piperidinyl]-2-oxypropyl]-4(3H)-quinazolinone derivative compounds in weight; wherein the ratio of the mixed solvent for the re-crystallization is: the mass ratio of alcohol:water:halohydrocarbon=1:0.1˜0.3:0.05˜0.2; wherein the alcohol used in the solvent for the re-crystallization is C1˜C4 alcohol; wherein the halohydrocarbon used in the solvent for the re-crystallization is dichromethane, trichloromethane, dichroethane or carbon tetrachloride.