化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 4-Hydroxy-o-toluic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Methyl 2-methyl-4-trimethylsilyloxybenzoate | HCID 21879730 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Hydroxy-o-toluic acid | HCID 68475 | 31.6% |
反応手順
A 100 mL round bottom flask equipped with magnetic stir bar was charged with 5.7 g methyl 2-methyl-4-trimethylsilyloxybenzoate and 2.0 g LiOH in 40 mL methanol and 10 mL water. After 2 hours at reflux the reaction was poured into 10 mL concentrated HCl and then 100 g ice. Extraction with ethyl acetate followed by concentration in vacuo gave a crude solid (70:30) product:starting material. Flash Chromatography using 50—50 ethyl acetate/hexanes as an eluent gave 1.15 g 2-methyl-4-hydroxybenzoic acid, m/e=193 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06924286B1 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-ba945a1148974ebd8c2017998c917847 |
| 出典メモ | uspto-grants-2005_08 |