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Acetic Acid → HCID 67791408、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | beta-Oxo-2-naphthalenepropanenitrile | HCID 222856 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | Methylamine hydrochloride | HCID 6364545 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 67791408 | HCID 67791408 | 58% |
反応手順
A solution of β-oxo-2-naphthalenepropionitrile (5.0 g, 0.0256 mol) in toluene is treated with methylamine hydrochloride ()2.6 g, 0.0384 mol), sodium acetate (3.15 g, 0.0386 mol) and a catalytic amount of acetic acid, heated at reflux temperature (fitted with a Dean Stark trap) for 6 hours, cooled, diluted with ethyl acetate and dilute hydrochloric acid. The organic phase is dried over Na2SO4 and concentrated in vacuo to give a residue which is triturated under hexanes to give the title compound as a yellow solid, 3.1 g (58% yield) mp 138° C., identified by IR, 1NHMR and mass spectral analyses.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05128485 |
| 出典データセット | uspto-grants-1992_07 |
| ORD ID | ord-d94f2da5002f430b99c1aeca0fbae274 |
| 出典メモ | uspto-grants-1992_07 |