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Acetonitrile → 4-Methoxybenzoylacetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Methyl anisate | HCID 8499 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Methoxybenzoylacetonitrile | HCID 233398 | — |
反応手順
166.2 grams (1 mole) of 4-methoxybenzoic acid methyl ester and 60 grams (2 moles) of sodium hydride (80 weight % suspension in white oil) were heated to 65° C. in 750 ml of dry toluene. Within 2 hours there were dropped in 82.1 grams (2 moles) of acetonitrile at 85° C. and then stirring was continued for a further 20 hours at 90° C. The precipitate was filtered off with suction, 200 ml of glacial acetic acid slowly stirred in with cooling and subsequently the mixture was added to 1 liter of ice water. The precipitated crystal mass was filtered off with suction, post washed with water and recrystallized from acetone. There were thus obtained 149 grams (85% of theory) or 4-methoxybenzoylacetonitrile having a melting point of 127°-129° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04728743 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-8b9db9372cc940d09b7f940dbb150c16 |
| 出典メモ | uspto-grants-1988_03 |