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Potassium Carbonate → HCID 58276234、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-(3-Bromophenyl)-1H-1,2,4-triazole | HCID 12461546 | — |
| 反応物 | 4-Chloro-2,2-dimethylbutanoate | HCID 21753047 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 58276234 | HCID 58276234 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822518B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-6b23d8ffbd59492aa20d8b1a464ad044 |
| 出典メモ | uspto-grants-2014_09 |