関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Urea | HCID 1176 | — |
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | Acetoacetamide | HCID 80077 | — |
| 反応物 | 3,5-Bis(trifluoromethyl)benzaldehyde | HCID 136247 | — |
| 触媒 | Cupric Chloride | HCID 24014 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(3,5-Bis-trifluoromethylphenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylic acid amide | HCID 86586005 | 36.2% |
反応手順
A mixture of 3,5-bis(trifluoromethyl)benzaldehyde (2.42 g, 10.0 mmol), acetoacetamide (1.01 g, 10.0 mmol), urea (0.90 g, 15.0 mmol), copper chloride (0.1 g, 1.0 mmol), boron trifluoride etherate (0.09 mL), AcOH (0.04 mL), and THF (20 mL) was heated at 65° C. for 18 h and cooled to room temperature. The resulting precipitates were collected by vacuum filtration, washed with THF, and air dried to give the title compound as an off-white solid(1.33 g, 36%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06809102B2 |
|---|
| 出典データセット | uspto-grants-2004_10 |
|---|
| ORD ID | ord-b6dad4d14dd3474a9e23c7ce406e1919 |
|---|
| 出典メモ | uspto-grants-2004_10 |
|---|
