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Diethyl Malonate → Diethyl 2,4,5-trimethoxybenzylidenemalonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 2,4,5-Trimethoxybenzaldehyde | HCID 20525 | — |
| 触媒 | Benzoic Acid | HCID 243 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Diethyl 2,4,5-trimethoxybenzylidenemalonate | HCID 13103748 | 87.8% |
反応手順
In 80 ml of toluene is dissolved 5.9 g of 2,4,5-trimethoxybenzaldehyde, followed by addition of 4.8 g of diethyl malonate, 0.3 ml of piperidine and 0.3 g of benzoic acid. The mixture is heated under reflux for 4 hours, water being removed via an ester tube. After cooling, the solvent is distilled off under reduced pressure and the residual crystals are recovered by filtration with n-hexane to give 8.9 g (87.3%) of diethyl 2,4,5-trimethoxybenzylidenemalonate, m.p. 86°-87° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04376777 |
| 出典データセット | uspto-grants-1983_03 |
| ORD ID | ord-6f93c1aa4d9b48f088f2bd32e5d97be1 |
| 出典メモ | uspto-grants-1983_03 |