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4-Fluorobenzaldehyde → 3-Methyl 5-ethyl 1,4-dihydro-2,4-di-(4-fluorophenyl)-6-isopropylpyridine-3,5-di-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Fluorobenzaldehyde | HCID 68023 | — |
| 反応物 | Methyl 4-fluorobenzoylacetate | HCID 579425 | — |
| 反応物 | Ethyl 3-amino-4-methyl-pent-2-enoate | HCID 59557418 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 生成物 | 3-Methyl 5-ethyl 1,4-dihydro-2,4-di-(4-fluorophenyl)-6-isopropylpyridine-3,5-di-carboxylate | HCID 15817268 | — |
反応手順
31 g (0.25 mol) of p-fluorobenzaldehyde, 49 g (0.25 mol) of methyl 4-fluorobenzoylacetate and 39.25 g (0.25 mol) of ethyl 3-amino-4-methyl-pent-2-enoate are boiled under reflux for 18 hours in 150 ml of ethylene glycol at a bath temperature of 130° C. The mixture is cooled to room temperature, extracted three times using 300 ml of diethyl ether, the combined ether phases are concentrated, and the residue is dissolved in 100 ml of toluene and chromatographed on 700 ml of silica gel (0.04-0.063 mm) using toluene as an eluent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06127383 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-bd915f11a9484b1ea6f258a9e7c239f8 |
| 出典メモ | uspto-grants-2000_10 |