化工社化工社 化学情報印刷レポート · 研究参考用
4,4,4-Trifluoro-1-(4-trifluoromethylphenyl)-1,3-butanedione → 3-Bromo-7-trifluoromethyl-5-(4-trifluoromethyl-phenyl)-pyrazolo[1,5-a]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4,4,4-Trifluoro-1-(4-trifluoromethylphenyl)-1,3-butanedione | HCID 10859020 | — |
| 反応物 | HCID 178509245 | HCID 178509245 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Bromo-7-trifluoromethyl-5-(4-trifluoromethyl-phenyl)-pyrazolo[1,5-a]pyrimidine | HCID 71539679 | 90% |
反応手順
A stirred mixture of commercially available 3-amino-4-bromo-pyrazole (14.00 g, 86.4 mmol) and 4,4,4-trifluoro-1-(4-trifluoromethyl-phenyl)-butane-1,3-dione (Example C.1 step 1) (24.56 g, 86.4 mmol) in acetic acid (170 mL) was heated under reflux conditions for 2.5 h. The reaction mixture was cooled to room temperature, diluted with water (340 mL), the precipitate was filtered off, washed with water and dried in air at 60° C. to give the 3-bromo-7-trifluoromethyl-5-(4-trifluoromethyl-phenyl)-pyrazolo[1,5-a]pyrimidine (31.77 g, 90%) as a yellow solid. MS (EI) 410.0 [(M)+], 412.0 [(M+2)+]; mp 136° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08063048B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-35bc5fcb7b03488cbbcc9a17e8ef2443 |
| 出典メモ | uspto-grants-2011_11 |