化工社化工社 化学情報印刷レポート · 研究参考用
Bromine → Ethyl 3-bromo-2-oxocyclohexanecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Ethyl 2-oxocyclohexanecarboxylate | HCID 95543 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Ethyl 3-bromo-2-oxocyclohexanecarboxylate | HCID 121765 | — |
反応手順
To a solution of ethyl 2-oxocyclohexanecarboxylate (50 g, 0.29 mol) in CHCl3 (150 mL) there was slowly added bromine (47 g, 0.29 mol) at 0° C. under a blanket of nitrogen as inert gas dropwise over a period of 45 minutes and the resultant mixture was stirred for a period of 6 hours at 0° C. and then for 16 hours at room temperature. Air was then passed into the reaction solution over a period of 2 hours. The organic phase was washed with aqueous saturated NaHCO3 solution (2×15 mL) and aqueous saturated NaCl solution (3×20 mL). Following drying of the organic phase over Na2SO4 and filtration, the solvent was removed. The product ethyl 3-bromo-2-oxocyclohexanecarboxylate was obtained in a yield of 72.6 g (corresponding to 99% of theory).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07348347B2 |
| 出典データセット | uspto-grants-2008_03 |
| ORD ID | ord-0ef8df6ab1f342108347979d946b8734 |
| 出典メモ | uspto-grants-2008_03 |