Diethylcarbamyl-substituted thiazole dihydropyrimidine
A technology of alkyl and methylene, which is applied in the field of drugs for the composition, treatment and prevention of hepatitis B virus infection, and can solve problems such as side effects and rebound effects
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Embodiment 1
[0115] Ethyl 4-(2,4-dichlorophenyl)-2-(thiazol-2-yl)-6-methyl-1,4-dihydropyrimidine-5-carboxylate
[0116]
[0117] With 10.0g (57.1mmol) of2,4-dichlorobenzaldehyde, 7.4g (57.1mmol) ethyl acetoacetic acid, 9.3g (57.1mmol) 2-amidino-thiazole hydrochloride and 5.7g (69.5mmol) acetic acid Sodium was dissolved or suspended in 500ml of ethanol and boiled under reflux for 16 hours. Cool to room temperature, filter with suction, and wash the residue with water to remove inorganic salts. 11.8 g (52.5%) of the product were obtained. Melting point: 164-166°C.
Embodiment 2
[0119] Ethyl 6-bromomethyl 4-(2,4-dichlorophenyl)-2-(thiazol-2-yl)-1,4-dihydropyrimidine-5-carboxylate
[0120]
[0121] 8.0g (20.2mmol) ethyl 4-(2,4-dichlorophenyl)-2-(thiazol-2-yl)-6-methyl-1,4-dihydropyrimidine prepared in Example 1 -5-Carboxylate was added to 140ml of carbon tetrachloride and heated to 50°C under argon atmosphere to obtain a clear solution. At this temperature, 4.36 g (24.2 mmol) of N-bromosuccinimide were added and mixing was maintained at this temperature for 10 minutes. Cool immediately, filter under vacuum at room temperature, and concentrate under reduced pressure. The purity of the product detected by HPLC was higher than 90%, and it was used as the raw material for the next step.
[0122] Rf=0.68 (petroleum ether / ethyl acetate=8:2)
[0123] B. Preparation Examples
Embodiment 3
[0125] Ethyl 4-(2,4-dichlorophenyl)-2-(thiazol-2-yl)-6-(4-morpholinomethyl)-1,4-dihydropyrimidine-5-carboxylate
[0126]
[0127] 5.0 g of the newly prepared ethyl-6-bromomethyl-4-(2-chloro4-chlorophenyl)-2-(thiazol-2-yl)-1,4-dihydropyrimidine-5 -Carboxylate was added to 60ml of methanol to form a solution, mixed with 5 times the amount of morpholine, and stirred at room temperature for 30 minutes. The solution was diluted with water and extracted with ethyl acetate.
[0128] Yield: 4.1g
[0129] Melting point: 155-157°C.
[0130] R f =0.48 (petroleum ether / ethyl acetate=8:2)
[0131] The enantiomers obtained in Example 3 were separated on a chiral column (Daicel Chiralpak AS-H, mobile phase: n-hexane / ethanol=99 / 1)
[0132] The anti-HBV active compounds in Example 3 are all enantiomers with longer retention time.
[0133] The list of activity data of the compounds of the present invention is as follows:
[0134]
[0135] Treatment of Hepatitis B virus producing He...
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Abstract
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