4-(3-BROMOPHENYL)-4H-1,2,4-TRIAZOLE synthesis

Yield:375858-05-2 24.95%

Reaction Conditions:

in toluene at 120; for 4 h;

Steps:

18 Synthesis of compound 18.2.

To a suspension of 3-bromoaniline (2.0g, 11.62mmol, 1.0eq) in toluene (30mL) was added compound 18.1 (3.3g, 23.24mmol, 2.0eq) and reaction mixture was heated at 120°C for 24h. After completion of reaction, reaction mixture was concentrated under reduced pressure to obtain residue which was dissolved in saturated sodium bicarbonate solution and washed with hexane. Aqueous layer separated and acidified with 1N hydrochloric acid to pH~5-6 and extracted with ethyl acetate. Organic layer was combined, dried over sodium sulfate and concentrated under reduced pressure to obtain solid which was triturated with hexane to obtain pure 18.2. (0.650g, Yield: 24.95%). MS (ES): m/z 224.97 [M+H]⁺.

References:

WO2020/112937,2020,A1 Location in patent:Paragraph 00440