化工社化工社 化学情報印刷レポート · 研究参考用
Hydroxyamine hydrochloride → 2-(Cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 2-(Cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde | HCID 86626769 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(Cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde oxime | HCID 86626839 | 80.8% |
反応手順
To ethanol (30 ml) are added 2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde (6.8 g), hydroxylamine hydrochloride (1.66 g) and sodium acetate (1.95 g) and the mixture is stirred at room temperature overnight. Ethanol is removed by evaporating under reduced pressure and thereto is added chloroform and water, and the mixture is separated. 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=10:1→2:1) to give 2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde oxime (5.78 g). MS (m/z): 301 [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-01fe7a08450d465594e83a1a07750c00 |
| 出典メモ | uspto-grants-2011_03 |