化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Ethyl 4,4-diethoxy-3-oxobutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Ethyl diethoxyacetate | HCID 80169 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl 4,4-diethoxy-3-oxobutanoate | HCID 11138577 | — |
反応手順
To a solution of 40 g of ethyl diethoxyacetate (227 mmol) in 67 mL of ethyl acetate there are added under argon, in portions, 6 g of sodium (261 mmol). The reaction mixture is then stirred at ambient temperature for 48 hours. There are added 10 mL of methanol, and then the mixture is hydrolysed with 65 mL of water. The pH of the reaction mixture is adjusted to pH 6 by adding 1N aqueous HCl solution. The mixture is separated and then extracted with ethyl acetate. The organic phases are combined, washed with brine, dried over MgSO4, filtered and concentrated to dryness. The title product is obtained in the form of an oil which is used in the next Step without being otherwise purified.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09108983B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-d9f46fe1de924c79b33b08ca572d0fd7 |
| 出典メモ | uspto-grants-2015_08 |