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Benzoic Acid → HCID 67267624、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoic Acid | HCID 243 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 3-Pyridinecarboxaldehyde | HCID 10371 | — |
| 反応物 | tert-Butyl methyl malonate | HCID 2733872 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 67267624 | HCID 67267624 | 48% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863305B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-339ee568794649a79418bafe7076f999 |
| 出典メモ | uspto-grants-2011_01 |