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Ethyl 2-chloroacetoacetate → 5-Ethyl-2-methyl-nicotinic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl 2-chloroacetoacetate | HCID 11858 | — |
| 反応物 | Ethylacrolein | HCID 70203 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-Ethyl-2-methyl-nicotinic acid ethyl ester | HCID 14436626 | 43.2% |
反応手順
A mixture of ethacrolein (12.8 g 0.152 mole) and ammonium acetate (24.4 g 0.304 mole) in 50 cc acetonitrile is stirred at room temperature and a solution of ethyl 2-chloroacetoacetate (25 g 0.152 mole) in 30 cc acetonitrile is added dropwise over 15 minutes. The reaction mixture is heated at reflux for 16 hours, cooled, and partitioned between water and ethyl acetate. The organic phase is concentrated in vacuo and chromatographed on silica gel using 9:1 hexane-ethylacetate to afford 12.7 g of the title product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04723011 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-24c7674dbf2448ab81e3a4fd1d43e7e8 |
| 出典メモ | uspto-grants-1988_02 |