3-[(2R)-2-Amino-2-phenylethyl]-5-(2-fluoro-3-methoxyphenyl)-1-[[2-fluoro-6-(trifluoromethyl)phenyl]methyl]-6-methyl-2,4(1H,3H)-pyrimidinedione synthesis

3synthesis methods

Product Name:3-[(2R)-2-Amino-2-phenylethyl]-5-(2-fluoro-3-methoxyphenyl)-1-[[2-fluoro-6-(trifluoromethyl)phenyl]methyl]-6-methyl-2,4(1H,3H)-pyrimidinedione
CAS Number:830346-50-4
Molecular formula:C28H24F5N3O3
Molecular Weight:545.5

830346-51-5 Synthesis

Carbamic acid, N-[(1R)-2-[5-(2-fluoro-3-methoxyphenyl)-3-[[2-fluoro-6-(trifluoromethyl)phenyl]methyl]-3,6-dihydro-4-methyl-2,6-dioxo-1(2H)-pyrimidinyl]-1-phenylethyl]-, 1,1-dimethylethyl ester

830346-51-5
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3-[(2R)-2-Amino-2-phenylethyl]-5-(2-fluoro-3-methoxyphenyl)-1-[[2-fluoro-6-(trifluoromethyl)phenyl]methyl]-6-methyl-2,4(1H,3H)-pyrimidinedione

830346-50-4
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Yield:830346-50-4 98.7%

Reaction Conditions:

with hydrogenchloride in ethanol;lithium hydroxide monohydrate at 60;Reagent/catalyst;Solvent;Temperature;

Steps:

12-16 This embodiment provides a preparation method of intermediate 2

Take the refined intermediate 1 (60 g, 93 mmol) obtained in Example 1, dissolve it in 240 mL of ethanol, add 30 mL of concentrated hydrochloric acid, and heat to 60±5°C for reaction. TLC plate layer detects that the reaction of intermediate 1 is complete, and the heating is stopped. reaction.Concentrate the reaction solution until no obvious solvent flows out, cool down, add 500mL isopropyl acetate and 200mL water to the reaction solution, cool down to 0±5°C, slowly add 15% aqueous sodium hydroxide solution to adjust pH=89, stir , layered; the organic phase was washed with 300 mL of saturated brine, dried over anhydrous sodium sulfate, and concentrated to obtain 50 g of white solid, namely Elagoli Intermediate 2, with a yield of 98.7% and a purity of 99.95%.

References:

CN114685379,2022,A Location in patent:Paragraph 0090-0106

1150560-59-0 Synthesis