化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 4-Benzyl-4-hydroxy-2-ketoglutaric acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Oxaloacetic Acid | HCID 970 | — |
| 反応物 | Phenylpyruvic acid | HCID 997 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Benzyl-4-hydroxy-2-ketoglutaric acid | HCID 10171474 | 37% |
反応手順
After 16.23 g of potassium hydroxide (having a purity of 85% by weight) was dissolved in 48 ml of water, 5.0 g (30.5 mmol) of phenylpyruvic acid and 12.1 g (91.4 mmol) of oxalacetic acid were added to the resulting solution, for reaction at ambient temperature for 72 hours (about pH 13 at the start of the reaction). Using conc. hydrochloric acid, the reaction solution was adjusted to pH 2.2, and extracted in ethyl acetate. The organic layer was rinsed in aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate and concentrated to obtain the residue. The residue was recrystallized in ethyl acetate and toluene, to obtain 2.8 g (11.3 mmol) of 4-benzyl-4-hydroxy-2-ketoglutaric acid in crystal form.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07390909B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-699fd30199a843e5a8a3aecdad1280d0 |
| 出典メモ | uspto-grants-2008_06 |