Thiazolyl dihydropyrimidine compound as well as preparation method and application thereof
A dihydropyrimidine and compound technology, applied in the field of thiazolyl dihydropyrimidine compounds, can solve problems such as easy recurrence, inability to be cured, and unfixed course of treatment
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Embodiment 1
[0078] Example 1: 4-(2-chloro-4-fluorophenyl)-6-((3-(difluoromethyl)-3-hydroxyazetidin-1-yl)methyl)-2- Preparation of (thiazol-2-yl)-1,4-dihydropyrimidine-5-carboxylic acid methyl ester
[0079]
[0080] Step 1) Synthesis of compound 4-(2-chloro-4-fluorophenyl)-6-methyl-2-(thiazol-2-yl)-1,4-dihydropyrimidine-5-carboxylic acid methyl ester:
[0081]
[0082] The compound 2-(2-chloro-4-fluorobenzylidene)-3-oxobutanoic acid methyl ester (5.3g, 20.7mmol), 2-thiazole formamidine hydrochloride (2.6g, 15.9mmol) was dissolved in Add potassium acetate (3.1 g, 31.8 mmol) to trifluoroethanol (70 mL), replace with nitrogen three times, and heat to reflux at 80° C. overnight. After the reaction, cool, filter with suction, concentrate the reaction solution, and the residue is separated and purified by column chromatography (n-heptane / ethyl ester (v / v)=9 / 1) to obtain a yellow solid 4-(2-chloro-4- Fluorophenyl)-6-methyl-2-(thiazol-2-yl)-1,4-dihydropyrimidine-5-carboxylic acid methyl e...
Embodiment 2
[0093] Example 2: 4-(2-bromo-4-fluorophenyl)-6-((3-(difluoromethyl)-3-hydroxyazetidin-1-yl)methyl)-2- Preparation of (thiazol-2-yl)-1,4-dihydropyrimidine-5-carboxylic acid methyl ester
[0094]
[0095] The compound 4-(2-bromo-4-fluorophenyl)-6-(bromomethyl)-2-(thiazol-2-yl)-1,4-dihydropyrimidine-5-carboxylic acid methyl ester (195 mg, 0.398mmol) dissolved in CHCl 3 (20mL), add compound 3-(difluoromethyl)azetidin-3-ol (71mg, 0.437mmol), DIPEA (513uL, 3.98mmol), heat at 45°C and stir for 4h. After finishing the reaction, cool, concentrate the reaction solution, dissolve the residue with DCM (50mL), wash with water (50mL×3), extract the aqueous phase with DCM (50mL×2), combine the organic phases, and anhydrous Na 2 SO 4 Dry, filter with suction, concentrate the filtrate, and separate and purify the residue by column chromatography (PE / EA (v / v) = 1 / 1 to pure EA / MeOH (v / v) = 4 / 1), then use PE-EA Recrystallization afforded 4-(2-bromo-4-fluorophenyl)-6-((3-(difluoromethyl)-3-...
Embodiment 3
[0098] Example 3: 4-(2-chloro-4-fluorophenyl)-6-((3-hydroxy-3-methylazetidin-1-yl)methyl)-2-(thiazole-2 Preparation of -yl)-1,4-dihydropyrimidine-5-carboxylic acid methyl ester
[0099]
[0100] The compound 4-(2-chloro-4-fluorophenyl)-6-(bromomethyl)-2-(thiazol-2-yl)-1,4-dihydropyrimidine-5-carboxylic acid methyl ester (178 mg, 0.398mmol) dissolved in CHCl 3 (5mL), add compound 3-methylazetidin-3-ol (49mg, 0.398mmol), DIPEA (516mg, 3.98mmol), heat at 45°C and stir for 4h. After finishing the reaction, cool, concentrate the reaction solution, dissolve the residue with DCM (50mL), wash with water (50mL×3), extract the aqueous phase with DCM (50mL×2), combine the organic phases, and anhydrous Na 2 SO 4 Drying, suction filtration, concentration of the filtrate, separation and purification of the residue by column chromatography (PE / EA (v / v) = 1 / 1 to pure EA), and recrystallization with PE-EA to obtain light yellow solid 4-(2- Chloro-4-fluorophenyl)-6-((3-hydroxy-3-methylaz...
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