関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl formate | HCID 8025 | — |
| 反応物 | 2,4,6-Trimethylphenylacetonitrile | HCID 520698 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Hydroxy-2-(2,4,6-trimethylphenyl)acrylonitrile | HCID 70142818 | 98% |
反応手順
A solution of 2,4,6-trimethylphenylacetonitrile (75 g) and ethyl formate (67 g) in 225 ml absolute ethanol was treated with solid sodium ethoxide (36 g) in small portions over 10 minutes, with good stirring. The mixture was heated to 60° C. under nitrogen for 16 hours and allowed to cool to room temperature. The reaction mixture was poured into 1.2 liters of water, extracted with diethyl ether (3×200 ml). The aqueous phase was acidified with 6 M HCl to pH=1 and extracted with ethyl acetate. The ethyl acetate extract was washed with brine, dried over MgSO4 and concentrated, yielding 46 g (98%) of 3-hydroxy-2-(2,4,6-trimethylphenyl)acrylonitrile (intermediate 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06469166B2 |
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| 出典データセット | uspto-grants-2002_10 |
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| ORD ID | ord-a2936e20d7a5450b9be65c7a0abc9c71 |
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| 出典メモ | uspto-grants-2002_10 |
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