반응 #157475

반응 방정식

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

용매

MeCN

반응 조건

후처리

1. 1
   온도The mixture was cooled
2. 2
   여과solid was collected by filtration
3. 3
   농축the filtrate was concentrated in vacuo Residue from the filtaret
4. 4
   여과Solid was collected by filtration
5. 5
   세척washed with water (×3)
6. 6
   기타recrystallized from MeOH/water

실험 절차

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).

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