Adding a certain compound to certain chemical reactions, such as: 130049-82-0, 3-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidine-4-one, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, 130049-82-0, blongs to pyrimidines compound. Application In Synthesis of 3-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidine-4-one
Example 1 – Synthesis of 3-[2-[4-(6-fluoro-1,2-benzoisoxazol-3-yl)-1-piperidinyl]ethyl-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]-pyrimidin-4-one hydrochloride (Paliperidone hydrochloride) 6-Fluoro-3-(4-piperidinyl)-1,2-benzoisoxazole hydrochloride (300 g, 1.17 mols), 3-(chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (343 g, 1.40 mols) and triethylamine (272 g, 2.69 mols) are suspended in methanol (1.5 1) in a 3000 ml reactor under nitrogen atmosphere, and the reaction mixture is heated at reflux temperature for 18-20 h. Conversion to the product is checked by HPLC titre, obtaining a yield of 96.5% in solution. The mixture is concentrated to a residue. The so obtained product has an XRPD spectrum as shown in Figure 5, and a DSC thermogram as shown in Figure 6, which are characteristic of paliperidone crystalline Form I. The mixture is taken up with demineralised water (1.5 1) and 36.5% hydrochloric acid (113 g, 1.13 mols), obtaining a solution with a pH of 3-4. A solid then reprecipitates, and the mixture is cooled to 0C and filtered. The solid is washed with demineralised water cooled to 0-5C (2 x 150 ml), and then with acetone cooled to 0-5C (3 x 200 ml). The solid is dried in oven under reduced pressure at a temperature of 50C for 16-18h. 451 g of paliperidone hydrochloride is obtained, with a potentiometric titre of 99.9%, an argentimetric titre of 7.8%, 99.2% HPLC purity, and a total yield of 90%. The product has an XRPD spectrum as shown in Figure 1, and a DSC thermogram as shown in Figure 2.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,130049-82-0, its application will become more common.
Reference:
Patent; Dipharma Francis S.r.l.; EP2243780; (2010); A2;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia