참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Nitrobenzaldehyde | HCID 11101 | — |
| 반응물 | Acetoacetate | HCID 6971017 | — |
| 반응물 | 2-Cyanoethyl 3-aminocrotonate | HCID 13671410 | — |
| 촉매 | Piperidine | HCID 8082 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | HCID 86742032 | HCID 86742032 | 77.1% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04730052 |
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| 출처 데이터셋 | uspto-grants-1988_03 |
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| ORD ID | ord-4cf9e1f8e25540d2adad8a7c7a6e113c |
|---|
| 출처 메모 | uspto-grants-1988_03 |
|---|