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Chloroform → 2-Benzoyl-3-dimethylaminocrotononitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Benzoylacetonitrile | HCID 64799 | — |
| 反応物 | 1,1-Dimethoxyethyl(dimethyl)amine | HCID 87835 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-Benzoyl-3-dimethylaminocrotononitrile | HCID 14673977 | — |
反応手順
To a solution of 14.5 g. (0.10 m) of benzoylacetonitrile in 100 ml. of chloroform, cooled in an ice-salt bath, was added 13.3 g. (0.1 m) of N,N-dimethylacetamide dimethylacetal in 20 ml. chloroform. The reaction mixture was stirred in the ice-salt bath for 2 hours, then evaporated in vacuo to an orange oil. The oil was dissolved in 150 ml. benzene and passed through Magnesol®. The filtrate was evaporated and the oil thus obtained was dissolved in 50 ml. benzene to which pet ether was added until the solution became cloudy. The precipitate which formed upon cooling was collected. The solid was recrystallized twice from benzene-pet ether, with charcoal treatment to yield 5.8 g. (27%) of light yellow crystals, m.p. 105°-106° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04259256 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-084c675acf0944cf8cdefa7dd2e4ae02 |
| 出典メモ | uspto-grants-1981_03 |