反応 #157475

反応方程式

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

溶媒

MeCN

反応条件

後処理

1. 1
   温度The mixture was cooled
2. 2
   ろ過solid was collected by filtration
3. 3
   濃縮the filtrate was concentrated in vacuo Residue from the filtaret
4. 4
   ろ過Solid was collected by filtration
5. 5
   洗浄washed with water (×3)
6. 6
   その他recrystallized from MeOH/water

実験手順

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).

出典