7-chloro-5-Methyl-2-(trifluoroMethyl)-[1,2,4]triazolo[1,5-a]pyriMidine synthesis

Yield:885461-50-7 53.1%

Reaction Conditions:

with trichlorophosphate for 2 h;Reflux;

Steps:

3.3 Step 3:

[0098] Step 3: Phosphoryl chloride (5 mL) was added to 8 (0.3 g, 13.7 mmol) and the reaction mixture was heated toreflux for 2 h. The reaction mixture was cooled to 25°C and phosphoryl chloride was removed under reduced pressure.Crude product was quenched with crushed ice and neutralized with 10% NaHCO3 solution and extracted with ethyl acetate (2 x 5 mL). The combined organic layers were washed with brine solution, dried over Na2SO4 and concentratedunder reduced pressure. Crude product was purified by column chromatography using 15-25% pet. ether and ethylacetate to yield compound 5c, 7-Chloro-5-methyl-2-(trifluoromethyl) -[1,2,4]triazolo[1,5-a] pyrimidine (0.17 g, 53.1%).1H NMR (400 MHz, CDCl3): δ 7.27 (s, 1H), 2.78 (s, 3H).

References:

EP3072894,2016,A1 Location in patent:Paragraph 0098