関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Cyclopropanemethanamine, N-propyl- | HCID 117787 | — |
| 反応物 | 2-Fluoro-5-(trifluoromethyl)benzaldehyde | HCID 2734904 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(Cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde | HCID 86626769 | — |
反応手順
2-Fluoro-5-trifluoromethyl-benzaldehyde (5 g) and cyclopropylmethyl-propyl-amine (5.57 ml) is dissolved in toluene (50 ml), and thereto is added potassium carbonate (10.7 g) and the mixture is stirred at 120° C. overnight. The reaction solution is cooled to room temperature, and thereto are added ethyl acetate and water, and the mixture is separated, and the organic layer is washed with a saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=20:1) to give 2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde (6.8 g). MS (m/z): 286 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07906517B2 |
|---|
| 出典データセット | uspto-grants-2011_03 |
|---|
| ORD ID | ord-8f93997dcbdb447f8a57d88115625b54 |
|---|
| 出典メモ | uspto-grants-2011_03 |
|---|