Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzoic Acid → 2-Pyridin-3-ylmethylene-malonic acid tert-butyl ester methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzoic Acid | HCID 243 | — |
| 반응물 | Piperidine | HCID 8082 | — |
| 반응물 | 3-Pyridinecarboxaldehyde | HCID 10371 | — |
| 반응물 | tert-Butyl methyl malonate | HCID 2733872 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Pyridin-3-ylmethylene-malonic acid tert-butyl ester methyl ester | HCID 67267624 | 48% |
반응 단계
A mixture of pyridine-3-carboxaldehyde (2.72 g), propanedioic acid, 1,1-dimethylethyl methyl ester (4.42 g), piperidine (0.173 g) and benzoic acid (0.155 g) in benzene (100 ml) was heated at reflux with removal of water to a Dean-Stark trap for 12 hours. The cooled mixture was washed with bicarbonate solution, concentrated under vacuum and the residue was purified by column chromatography, eluting with ethyl acetate-hexane (3:7) to afford racemic 2-pyridin-3-ylmethylene-malonic acid tert-butyl ester methyl ester as an oil (3.21 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07863305B2 |
| 출처 데이터셋 | uspto-grants-2011_01 |
| ORD ID | ord-339ee568794649a79418bafe7076f999 |
| 출처 메모 | uspto-grants-2011_01 |