関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 4-(Trifluoromethyl)benzylamine | HCID 76804 | — |
| 反応物 | 5-Formyl-2-methoxybenzoic acid | HCID 3926683 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Formyl-2-methoxy-N-[[4-(trifluoromethyl)phenyl]methyl]-benzamide | HCID 12094661 | 78% |
反応手順
To a suspension of 1.00 g of 5-formyl-2-methoxybenzoic acid in 50 ml of methylene chloride were added 1.00 ml of triethylamine and 0.60 ml of ethyl chlorocarbonate, and the mixture was stirred for 15 minutes at room temperature. Then, a solution of 1.17 g of 4-trifluoromethylbenzylamine in 10 ml of methylene chloride was added and the mixture was stirred further for 3 hours at room temperature. After washed with water, the reaction mixture was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue obtained was purified by means of column chromatography (silica gel, hexane:ethyl acetate=1:1) and then recrystallized from a mixed solvent of diethyl ether-ethyl acetate-hexane to obtain 1.46 g of 5-formyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06706763B1 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-85c9d352781a4a668ba10aa38b2d8687 |
|---|
| 出典メモ | uspto-grants-2004_03 |
|---|