化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → (4-Nitrophenyl)methyl 4-chloro-3-oxobutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-Nitrobenzyl alcohol | HCID 69275 | — |
| 反応物 | 4-Chloro-3-oxobutyryl chloride | HCID 3016262 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (4-Nitrophenyl)methyl 4-chloro-3-oxobutanoate | HCID 20196963 | 104.3% |
反応手順
After 191.2 g (1.25 mol) of p-nitrobenzyl alcohol is dissolved in 250 ml of methylene chloride, 98.8 g of pyridine is added, and the mixture is cooled to -5° to 0° C. A solution of 193.75 g (1.25 mol) of γ-chloroacetoacetyl chloride (γ-CAC) in 431 ml of methylene chloride is added at the same temperature over an hour and, after completion of the addition, the mixture is stirred for 30 minutes. The resulting pyridine hydrochloride is filtered off. The filtrate and washings are combined and washed with 2 l-portions of water. The organic layer is dried over sodium sulfate and the solvent is then distilled off to give 354 g of p-nitrobenzyl γ-chloroacetoacetate as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04572801 |
| 出典データセット | uspto-grants-1986_02 |
| ORD ID | ord-bd0e50e137d3417da7d549a5d1eba38e |
| 出典メモ | uspto-grants-1986_02 |