化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Ethyl 6-(4-chlorophenyl)-2,4,6-trioxohexanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Oxalate | HCID 7268 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(4-Chlorophenyl)butane-1,3-dione | HCID 238083 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | Ethyl 6-(4-chlorophenyl)-2,4,6-trioxohexanoate | HCID 15578432 | — |
反応手順
A solution of 1-(4-chlorophenyl)-1,3-butanedione (0.6 g) and diethyl oxalate (0.83 ml) in 1,2-dimethoxyethane (2 ml) was added to a stirred suspension of sodium hydride (0.44 g, 50% dispersion in mineral oil, washed with petrol 40°-60° C.) in 1,2-dimethoxyethane (5 ml) under nitrogen. The stirred mixture was heated under reflux for 1 hour, cooled and acidified with 2M hydrochloric acid (10 ml). The brown solid which formed was recrystallised from ethanol-water to give the title product (mp 93°-94° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04448787 |
| 出典データセット | uspto-grants-1984_05 |
| ORD ID | ord-d64d2eb4bba64c0b8da63df92b365699 |
| 出典メモ | uspto-grants-1984_05 |