化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylammonium tetrafluoroborate → Ethyl 2-dimethylamino-6-(4-biphenylyl)-5-methylthio-6-oxo-2,4-hexadienoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylammonium tetrafluoroborate | HCID 140161 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | Ethyl 6-phenyl-6-oxo-5-methylthio-2-dimethylamino2,4-hexadienoate | HCID 44325574 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 2-dimethylamino-6-(4-biphenylyl)-5-methylthio-6-oxo-2,4-hexadienoate | HCID 54170142 | — |
反応手順
The procedure is as in Example 4 for the preparation of ethyl 6-phenyl-6-oxo-5-methylthio-2dimethylamino-2,4-hexadienoate, starting with N-(3-dimethylamino)-3-ethoxycarbonylpropenyldiene)-N-methylmethanaminium tetrafluoroborate (6 g), a 2M ethanolic solution of sodium ethylate (10.5 cc) and α-methylthio-4-phenylacetophenone (5.1 g) in ethanol (150 cc). After purification by chromatography on a silica column with a mixture of cyclohexane and ethyl acetate (50:50 by volume) as eluent, ethyl 2-dimethylamino-6-(4-biphenylyl)-5-methylthio-6-oxo-2,4-hexadienoate (2.8 g) is obtained in the form of an orange-coloured oil, and is used in the crude state in the subsequent syntheses.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04886835 |
| 出典データセット | uspto-grants-1989_12 |
| ORD ID | ord-71bc1b8e1b25490a8350181c257f760a |
| 出典メモ | uspto-grants-1989_12 |