化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 3-(4-Chloro-2-hydroxyphenyl)propanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,2-Dimethyl-1,3-dioxane-4,6-dione | HCID 16249 | — |
| 反応物 | 4-Chloro-2-hydroxybenzaldehyde | HCID 520101 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(4-Chloro-2-hydroxyphenyl)propanoic acid | HCID 67390445 | — |
反応手順
The subtitle compound was prepared by using the product from step i). (3.48 g) was added to a solution of triethylamine (10 ml) and formic acid (7 ml) in DMF (30 ml) after 20 minutes. Meldrum's acid (3.22 g) was added and the mixture heated to 100 C for 4 hours. The solution was basified with 2M NaOH, extracted with ether (discarded). The aqueous layer was acidified with 2M HCl, extracted with ethyl acetate, dried and concentrated under reduced pressure to give an oil. The residue was purified by chromatography on silica eluting with diethyl ether/isohexane 1:5, yield 0.40 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08022248B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-40b7d434de8745c08019deb28343aa4d |
| 出典メモ | uspto-grants-2011_09 |