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2,3-Dichloro-6-fluorobenzaldehyde → 3-Methyl 5-(1-methylethyl) 4-(2,3-dichloro-6-fluorophenyl)-2-(fluoromethyl)-1,4-dihydro-6-methyl-3,5-pyridinedicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3-Dichloro-6-fluorobenzaldehyde | HCID 3260062 | — |
| 反応物 | Isopropyl3-aminocrotonate | HCID 3271821 | — |
| 反応物 | Methyl 4-fluoro-3-oxobutanoate | HCID 14170515 | — |
| 生成物 | 3-Methyl 5-(1-methylethyl) 4-(2,3-dichloro-6-fluorophenyl)-2-(fluoromethyl)-1,4-dihydro-6-methyl-3,5-pyridinedicarboxylate | HCID 70089470 | 33.8% |
反応手順
2,3-Dichloro-6-fluorobenzaldehyde (1.44 g, 7.5 mmoles), methyl 4-fluoro-3-oxobutanoate (1.0 g, 7.5 mmoles) and 1-methylethyl 3-amino-2-butenoate (1.06 g, 7.5 mmoles) were heated at 90° under nitrogen with stirring for 2.5 hours. The cooled reaction mixture was chromatographed on silica eluting with ethyl acetate/methylene chloride mixtures. The title compound (1.1 g) was obtained by crystallisation from a petroleum ether (60°-80°)/2-propanol mixture mp 129°-31°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04686217 |
| 出典データセット | uspto-grants-1987_08 |
| ORD ID | ord-e30d54292b834134a4f513af2cb9a96d |
| 出典メモ | uspto-grants-1987_08 |