6-oxohexahydropyrimidine derivative, its preparation method and pharmaceutical application
A compound and general formula technology, applied in the field of medicinal chemistry, can solve the problems of general activity and single structure type, and achieve the effect of potential medicinal value
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Embodiment 1
[0078] 3-(3,3-Dimethylbutyryl)-N-(4-(4-methylthiazol-5-yl)benzyl)-6-oxohexahydropyrimidine-4-carboxamide
[0079]
[0080] Step 1: 4-(4-Methylthiazol-5-yl)benzonitrile
[0081] Add KOAc (3.2g) and 4-methylthiazole (3.24g) to a 50ml single-necked bottle, add 15ml DMF to dissolve, add p-bromoxynil (3.0g), add Pd(OAc) 2 (16 mg), heated under reflux and stirred in an external bath, after 10 hours, TLC detected that the raw materials were completely reacted, filtered, added 50 ml of water, extracted three times with EA (20 mL×3), combined the organic phases, washed with 50 ml of saturated aqueous sodium chloride solution, anhydrous sulfuric acid Dry over sodium, filter, and concentrate the filtrate under reduced pressure to obtain 3.2 g of the title compound.
[0082] Step 2: (4(4-methylthiazol-5-yl)phenyl)methanamine
[0083] Add 4-(4-methylthiazol-5-yl)benzonitrile (2.0g) into a 50ml three-necked flask, add 15ml of methanol to dissolve, add Raney nickel, replace with hydroge...
Embodiment 2
[0093] N-([1,1'-biphenyl-4-methyl)-3(3,3-dimethylbutyryl)-6-oxohexahydropyrimidine-4-carboxamide]
[0094]
[0095] Step 1: N-([1,1'-biphenyl-4-methyl)-3(3,3-dimethylbutyryl)-6-oxohexahydropyrimidine-4-carboxamide]
[0096] Add the 3-(3,3-dimethylbutyryl)-6-oxahexahydropyrimidine-4-carboxylic acid (150 mg) prepared above into a 25 ml one-mouth bottle, add 5 ml of DMF, and add HBTU (250 mg) , add 1,1'-biphenyl-4-methylaminoamine (114mg), add DIPEA (240mg), stir at room temperature for 3h, LC-MS detects that the reaction is complete. Add 15ml of water, extract the aqueous phase with EA (20mL×3), combine the organic phases, wash with 50ml of saturated aqueous sodium chloride solution, and dry over anhydrous sodium sulfate. It was filtered and concentrated under reduced pressure to obtain 185 mg of an oily substance, which was prepared by HPLC to obtain 35 mg of the title compound (HPLC purity: 97.6%).
[0097] The rest of the reaction steps were prepared with reference to th...
Embodiment 3
[0101] 3-(3,3-Dimethylbutyryl)-N-(4-hydroxybenzyl)-6-oxohexahydropyrimidine-4-carboxamide
[0102]
[0103] Step 1: 3-(3,3-Dimethylbutyryl)-N-(4-hydroxybenzyl)-6-oxohexahydropyrimidine-4-carboxamide
[0104] Add the 3-(3,3-dimethylbutyryl)-6-oxahexahydropyrimidine-4-carboxylic acid (150 mg) prepared above into a 25 ml one-mouth bottle, add 5 ml of DMF, and add HBTU (250 mg) , add (4-hydroxyphenyl)methanamine (78.12mg), add DIPEA (240mg), stir at room temperature for 3h, LC-MS detects that the reaction is complete. Add 15ml of water, extract the aqueous phase with EA (20mL×3), combine the organic phases, wash with 50ml of saturated aqueous sodium chloride solution, and dry over anhydrous sodium sulfate. It was filtered and concentrated under reduced pressure to obtain 170 mg of an oily substance, which was prepared by HPLC to obtain 25 mg of the title compound (HPLC purity: 96.4%).
[0105] The rest of the reaction steps were prepared with reference to the synthesis method...
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