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3-Nitrobenzaldehyde → Nicardipine Impurity 19
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Nitrobenzaldehyde | HCID 7449 | — |
| 反応物 | Acetoacetate | HCID 6971017 | — |
| 反応物 | 2-Cyanoethyl 3-aminocrotonate | HCID 13671410 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Nicardipine Impurity 19 | HCID 10429284 | 88.4% |
反応手順
10.3 g of 3-nitratopropyl acetoacetate, 7.7 g of 2-cyanoethyl 3-aminocrotonate and 7.6 g of 3-nitrobenzaldehyde in 76 ml of isopropyl alcohol were heated at reflux for 6.5 hours, and cooled on ice. The crystals which precipitated were collected by filtration, dried, applied to a silica gel column chromatography (eluent: dichloromethane) and recrystallized from ethanol to give 16.4 g of 2,6-dimethyl-4-(3-nitrophenyl)1,4-dihydropyridine-3,5-dicarboxylic acid 3-(2-cyanoethyl) ester 5-(3-nitratopropyl) ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04730052 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-cf05da0d5c2c4a7cb1ab8b92df4a8cd5 |
| 出典メモ | uspto-grants-1988_03 |