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Triethylamine → 2-(3-Phenoxybenzoyl)-3-dimethylaminoacrylonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-(Dimethylamino)prop-2-enenitrile | HCID 97497 | — |
| 反応物 | 3-Phenoxybenzoyl chloride | HCID 2760341 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-(3-Phenoxybenzoyl)-3-dimethylaminoacrylonitrile | HCID 54099632 | 36.2% |
反応手順
A mixture of 3-phenoxybenzoyl chloride (6.9 g), 3-dimethylaminoacrylonitrile (2 g) and triethylamine (4 g) in dry dioxan (50 ml) was refluxed for 6 hours under a nitrogen atmosphere. After standing at room temperature overnight, the dioxan was evaporated in vacuo and dichloromethane added to the residue. The extracts were washed with water, 2N NaOH, brine and finally dried over MgSO4. After filtration and evaporation of the dichloromethane, the residue was purified on a silica gel column using 5% methanol-dichloromethane as eluant to give the title compound (2.2 g, 36%) as a white solid of m.p. 80°-82° C. (identical to that described in Example 46).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05152825 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-30ba1b7a3a6a4330b33d69566dcace07 |
| 出典メモ | uspto-grants-1992_10 |