Reaktion #303093

Reaktionsgleichung

3-(2-Bromo-2-methylpropionylamino)propionic acid methyl ester

3-(4-chloro-2-fluoro-5-hydroxyphenyl)-1-methyl-6-trifluoromethyl-1H-pyrimidin-2,4-dione

K2CO3

→

compound

Ausbeute 63.8%

3-[{2-[2-chloro-5-(3,6-dihydro-3-methyl-2,6-dioxo-4-trifluoromethyl-1(2H)-pyrimidinyl)-4-fluorophenoxy]-1-oxoisobutyl}amino]propionic acid methyl ester

Ausbeute 63.8%

Lösungsmittel

acetonitrile

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe reaction mixture was heated for 12 hours
2. 2
   Temperaturunder reflux
3. 3
   Temperaturcooled
4. 4
   WaschenAfter washing with water (50 mL), thus obtained organic layer
5. 5
   Trocknenwas dried with magnesium sulfate
6. 6
   Einengenconcentrated
7. 7
   SonstigeThe concentrate was purified by silica gel column chromatography

Vorschrift

3-(2-Bromo-2-methylpropionylamino)propionic acid methyl ester (224 mg) and 3-(4-chloro-2-fluoro-5-hydroxyphenyl)-1-methyl-6-trifluoromethyl-1H-pyrimidin-2,4-dione (250 mg) were dissolved in acetonitrile 5 ml. After addition of K2CO3 (204 mg), the reaction mixture was heated for 12 hours under reflux, cooled and diluted with ethyl acetate (50 mL). After washing with water (50 mL), thus obtained organic layer was dried with magnesium sulfate and concentrated. The concentrate was purified by silica gel column chromatography to give the target compound (240 mg).

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