関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Nitrobenzaldehyde | HCID 11101 | — |
| 反応物 | Acetoacetate | HCID 6971017 | — |
| 反応物 | 2-Cyanoethyl 3-aminocrotonate | HCID 13671410 | — |
| 触媒 | Piperidine | HCID 8082 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | HCID 86742032 | HCID 86742032 | 77.1% |
反応手順
9.7 g of 2-nitratoethyl acetoacetate, 7.6 g of 2-nitrobenzaldehyde and 0.2 g of piperidine in 40 ml of benzene were heated at reflux under azeotropic dehydration conditions for 3 hours. The mixture was treated in a manner similar to that of Referential Example 1, there was obtained the residue, to which was added 7.7 g of 2-cyanoethyl 3-aminocrotonate. The mixture was taken up in 40 ml of isopropyl alcohol and heated at reflux for 3 hours. The isopropyl alcohol was evaporated under reduced pressure, and the residue was applied to a silica gel column chromatography (eluent: dichromomethane) and recrystallized from a mixture of dichromethane and diethyl ether to give 14.3 g of 2,6-dimethyl-4-(2-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid 3-(2-cyanoethyl) ester 5-(2-nitratoethyl) 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-4cf9e1f8e25540d2adad8a7c7a6e113c |
|---|
| 出典メモ | uspto-grants-1988_03 |
|---|