関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1-Dimethoxyethyl(dimethyl)amine | HCID 87835 | — |
| 反応物 | p-Fluorobenzoylacetonitrile | HCID 2783172 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-(p-Fluorobenzoyl)-3-dimethylaminocrotononitrile | HCID 23468497 | — |
反応手順
To a solution of 1.6 g. of p-fluorobenzoylacetonitrile [Pihl et al., Reakts. Sposobnost Org. Soedin. Tartu. Gos. Univ., 5 (1), 27, (1968)] in 30 ml. of chloroform, cooled to -10° C., is added 1.4 g. of N,N-dimethylacetamide dimethylacetal. The reaction mixture is stirred at -10° C. for 2 hours and then evaporated in vacuo to an oil. This oil is dissolved in 150 ml. of benzene and filtered through Magnesol®. The filtrate is evaporated to 50 ml. and petroleum ether is added to effect crystallization. The product is collected by filtration and then recrystallized from benzene-petroleum ether with charcoal treatment giving the desired product.
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-7c5808a82e174b9fa1fa2e1ca3f810ae |
|---|
| 出典メモ | uspto-grants-1981_03 |
|---|