In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 130049-82-0, 3-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidine-4-one, other downstream synthetic routes, hurry up and to see.
Related Products of 130049-82-0, Adding some certain compound to certain chemical reactions, such as: 130049-82-0, name is 3-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidine-4-one,molecular formula is C11H15ClN2O2, 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.
Into a clean 2L, three-necked RB flask equipped with shaft, condenser, and thermo socket was charged 600 ml of DMF, lOOg (0.404 moles) of 3-(2-Chloroethyl)-6,7,8,9- tetrahydro-9-hydroxy-4H-pyrido[l52-a]pyrimidin-4-one of formula- VI obtained from Example 5, 67.19g (0.404 moles) of potassium iodide, 111.91g (0.808moles) of potassium, carbonate and 103.68g (0.404 moles) of 6- fluoro-3-(4- piperidinyl)-l,2- benzisoxazole HCl (formula-VII). The reaction mass was heated to 60-650C and maintained for 18h. Reaction mass was cooled to 25-300C, stirred for Ih and filtered under vacuum. The wet cake was washed with 200ml of DMF. The wet cake was leached with 2 x 500ml of water and 1 x 500ml of methanol. The wet material was dried in the oven at 70-750C for Ih to yield 114g of technical grade paliperidone. Above technical grade paliperidone was recrystallized from methanol via charcoal treatment to get 6Og (34.74% yield) of pure paliperidone. Purity by HPLC is > 99.8%.S Alternatively technical grade paliperidone was purified by the following chemical method.Above technical grade paliperidone (114g) was dissolved in 6.84L of methanol at 65- 7O0C. Charcoal (20 g) was added to the resultant solution and filtered under vacuum using a filter aid. The solvent was distilled of from the filtrate at 60-650C using0 rotavapor under vacuum to get a cream colored solid. Methanol (575 ml) was added to the solid and stirred for 45min at 25-300C. The reaction mass was filtered and dried in an oven at 70-750C to get 90 g of paliperidone.Into a clean and dry IL, three-necked RB flask equipped with shaft, thermo socket,5 addition funnel and stopper was charged 57.0 ml of cone. HCl and 570 ml of water.The reaction mass was stirred for 5min and charged the above solid (9Og). The reaction mass was stirred for 5-10min at 25-300C to get yellow colored clear liquid. pH of the reaction mass was adjusted to 6.0 to 6.5 by dropwise addition of dilute(concentrated aq ammonia solution was diluted with equal volume of water) aq.0 ammonia solution. The reaction mass was stirred for 30min and filtered under vacuum. The wet solid was dried in the oven at 70-750C to get 88g of paliperidoneHCl.Above solid was transferred taken into a IL RB flask containing 570 ml of methanol.5 The suspension was stirred for 30min at 25-3O0C, filtered under vacuum and dried in the oven at 70-750C for Ih to get 85 g pure paliperidone HCl. HPLC purity is > 99.80%.Above paliperidone HCl salt (85.0 g) and 2280 ml of water were suspended in a RB0 flask at 25-300C. pH was adjusted to 8.5 to 9.0 by adding aq. potassium carbonate solution (prepared from 57 g of potassium carbonate and 570 ml of water). The resultant cream-colored suspension was stirred for 30 min at 25-300C and filtered under vacuum. The wet cake was washed with 1500ml of water followed by 300ml of methanol. The wet cake was triturated with 450 ml of methanol for 30 min and filtered. Paliperidone was dried in vacuum oven at 65-70C for 4h to afford 59 g (34.33%) of pure paliperidone. Purity by HPLC is > 99.8%. 1H-NMR (CDCl3): 1.75 (m, 2H, aliphatic-H), 1.95 (m, IH, aliphatic-H), 2.15 (m, 5H, aliphatic-H), 2.24 -2.40 (m, 5H, aliphatic-H), 2.56 (t, 2H, -CH2-, J = 6.84 Hz), 2.76 (t, 2H, -CH2-, J = 7.82 Hz), 3.09 (m, IH, aliphatic-H), 3.18 (d, 2H, aliphatic-H, J =11.72 Hz), 3.92 (m, 2H, aliphatic-H), 4.15 (s, IH, -OH, D2O exchangeable), 4.50 (dd, IH, aliphatic-H J = 3.91 Hz), 7.07 (m, IH, aromatic-H), 7.23 (m, IH aromatic-H), 7.70 (dd, IH, aromatic-H, J= 2.93 Hz).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 130049-82-0, 3-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidine-4-one, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; NATCO PHARMA LIMITED; WO2009/10988; (2009); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia