Reaktion #157475

Reaktionsgleichung

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

Lösungsmittel

MeCN

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was cooled
2. 2
   Filtrationsolid was collected by filtration
3. 3
   Einengenthe filtrate was concentrated in vacuo Residue from the filtaret
4. 4
   FiltrationSolid was collected by filtration
5. 5
   Waschenwashed with water (×3)
6. 6
   Sonstigerecrystallized from MeOH/water

Vorschrift

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).

Quelle