3-(2-Chloroethyl)-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one synthesis
- Product Name:3-(2-Chloroethyl)-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one
- CAS Number:63234-80-0
- Molecular formula:C11H15ClN2O
- Molecular Weight:226.7
![3-(2-Chloroethyl)-2-methylpyrido[1,2-a]pyrimidin-4-one](/CAS/GIF/41078-70-0.gif)
41078-70-0
63234-80-0
The general procedure for the synthesis of 3-(2-chloroethyl)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one from 3-(2-chloroethyl)-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one is as follows: 28 g of 3-(2-chloroethyl)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one obtained in step A) was dissolved in 90 mL 6N hydrochloric acid. -a]pyrimidin-4-one was dissolved in 90 mL of 6N hydrochloric acid, followed by the addition of 2.8 g of 10% palladium carbon catalyst to the solution. The reaction mixture was subjected to 35 psi hydrogen pressure and hydrogenated at room temperature with stirring for 8 hours. Upon completion of the reaction, the mixture was filtered through diatomaceous earth (Cellite) to remove the catalyst. The filtrate was concentrated under reduced pressure to give a residue. To the residue was added 200 mL of isopropanol and the mixture was stirred. The precipitated solid was collected by filtration and dried to give 25.1 g of the target product 3-(2-chloroethyl)-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one as white crystals in 90% yield.
41078-70-0
138 suppliers
$27.00/5g
63234-80-0
276 suppliers
$6.00/1g
Yield:63234-80-0 90%
Reaction Conditions:
with hydrogenchloride;hydrogen;palladium in water at 20; under 1810.07 Torr; for 8 h;
Steps:
2. B B) Preparation of 3- (2-chloroethyl)-6, 7,8, 9-tetrahydro-2-methyl-4H-pyrido [1, 2- a] pyrimidin-4-one
28g of [3- (2-CHLOROETHYL)-2-METHYL-4H-PYRIDO [1,] 2-a] pyrimidin-4-one obtained in step A) was dissolved in [90ML] of 6N hydrochloric acid, 2.8g of 10%- palladium was added thereto, and then the mixture was hydrogenated under a hydrogen pressure of 35psi at room temperature for 8 hours. The reaction mixture was filtered through Cellite and the filtrate was concentrated under a reduced pressure, [200ML] of isopropanol was added to the residue, and then the mixture was stirred. The solid was filtered and dried to obtain 25. 1g of the title compound as a white crystal (yield: 90%).
References:
HANMI PHARM. CO., LTD. WO2004/35573, 2004, A1 Location in patent:Page 9
504-29-0
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$5.00/5 g
63234-80-0
276 suppliers
$6.00/1g
517-23-7
452 suppliers
$5.00/25g
63234-80-0
276 suppliers
$6.00/1g