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4,4,4-Trifluoro-1-phenyl-1,3-butanedione → Ethyl 5-phenyl-7-(trifluoromethyl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4,4,4-Trifluoro-1-phenyl-1,3-butanedione | HCID 67589 | — |
| 反応物 | HCID 178469928 | HCID 178469928 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Ethyl 5-phenyl-7-(trifluoromethyl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine-3-carboxylate | HCID 135568187 | 79% |
反応手順
A mixture of 4,4,4-trifluoro-1-phenyl-1,3-butanedione 1 (6.97 g, 32.24 mmol) and ethyl 3-aminopyrazole-4-carboxylate 2 (5.0 g, 32.22 mmol) in AcOH (100 mL) was refluxed for 4 h. The mixture was cooled to room temperature and concentrated and precipitated crystals were collected by filtration to give 8.63 g (79%) of the title compound as yellow crystals. 1H NMR (CDCl3, 200 MHz): 1.47 (3H, t, J=7.0 Hz), 4.47 (2H, q, J=7.0 Hz), 7.54-7.61 (3H, m), 7.80 (1H, s), 8.23-8.28 (2H, m), 8.68 (1H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447100B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-58eb9390806a4d3ca9174761fd102990 |
| 出典メモ | uspto-grants-2016_09 |