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Methanol → Methyl 3-hydroxy-4-methoxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Isovanillic Acid | HCID 12575 | — |
| 生成物 | Methyl 3-hydroxy-4-methoxybenzoate | HCID 4056967 | — |
反応手順
A mixture of 50.0 g of 3-hydroxy-4-methoxybenzoic acid in 500 ml of absolute methyl alcohol containing 2.5 ml of concentrated sulfuric acid, is heated at reflux temperature for 6 hours. The reaction is concentrated in vacuo, 250 ml of ice water is added and the residue is extracted with diethyl ether. The organic layers are washed with saturated sodium bicarbonate and saturated sodium chloride, dried and concentrated in vacuo. The residue is dissolved in diethyl ether, passed through a pad of silica gel and concentrated in vacuo. The solid is recrystallized from diethyl ether/hexane to give 33 g of the desired product as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05208247 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-2ee6acfb6e34422abcb614110227ce74 |
| 出典メモ | uspto-grants-1993_05 |