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Piperidine → Methyl 2-(2-cyanobenzylidene)-4,4-dimethoxyacetoacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 2-Cyanobenzaldehyde | HCID 101209 | — |
| 反応物 | Methyl 4,4-dimethoxy-3-oxobutanoate | HCID 11008445 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Methyl 2-(2-cyanobenzylidene)-4,4-dimethoxyacetoacetate | HCID 53675930 | 36.8% |
反応手順
A benzene solution (120 ml) of 2-cyanobenzaldehyde (30.97 g), methyl 4,4-dimethoxyacetoacetate (46.14 g), acetic acid (2.3 g) and piperidine (2.4 g) was refluxed under heating for 8 hours. After addition of benzene (80 ml) and washing with water, the solution was treated with an activated charcoal. The evaporated residue was chromatographed on silica gel (500 g) with methylene chloride as an eluent. The fractions containing a desired compound were collected and evaporated to give methyl 2-(2-cyanobenzylidene)-4,4-dimethoxyacetoacetate (25.16 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04370334 |
| 出典データセット | uspto-grants-1983_01 |
| ORD ID | ord-99218264995843b0a09f087139738dcf |
| 出典メモ | uspto-grants-1983_01 |