Reacción #157475

Ecuación de reacción

3-(3-bromophenyl)-1H-1,2,4-triazole

K2CO3

chloromethylpivalate

→

title compound

[3-(3-Bromophenyl)-1H-1,2,4-triazol-1-yl]methyl 2,2-dimethylpropanoate

Disolventes

MeCN

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe mixture was cooled
2. 2
   Filtraciónsolid was collected by filtration
3. 3
   Concentraciónthe filtrate was concentrated in vacuo Residue from the filtaret
4. 4
   FiltraciónSolid was collected by filtration
5. 5
   Lavadowashed with water (×3)
6. 6
   Otrorecrystallized from MeOH/water

Procedimiento

A slurry of 3-(3-bromophenyl)-1H-1,2,4-triazole (58.5 g; 261 mmol; Step 1 above), anhydrous K2CO3 (43.2 g; 313 mmol), and chloromethylpivalate (45 mL; 313 mmol) in dry MeCN (250 mL) was heated to 80° C. (Note 1) for 1 hour. The mixture was cooled, solid was collected by filtration and the filtrate was concentrated in vacuo Residue from the filtaret was combined with the filtered solid and the whole was stirred with water approximately 20 minutes. Solid was collected by filtration, washed with water (×3) and recrystallized from MeOH/water, affording the title compound as a colorless solid. LC/MS (method E) tR 0.88 min, m/z 338, 340 (M+H, Br isotopes).

Fuente