関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methyl 2-methoxy-2'-methylbiphenyl-4-carboxylate | HCID 53941402 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Methoxy-4-(2-methylphenyl)benzoic acid | HCID 18001076 | 87.3% |
反応手順
To the 2-methoxy-2′-methyl-biphenyl-4-carboxylic acid methyl ester of step C (26 mmol) was added methanol (10 mL), tetrahydrofuran (45 mL) and 1 N sodium hydroxide (33 mL). The solution was refluxed vigorously in an oil bath at 105° C. for one hour. The volatile solvents were evaporated and the solution was chilled in ice. 2N hydrochloric acid was added until the pH was ˜1. The product was extracted into ethyl acetate, dried with anhydrous magnesium sulfate, and evaporated to a white solid. This was recrystallized from ethyl acetate/hexane to afford 5.5 g of title compound (86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07691848B2 |
|---|
| 出典データセット | uspto-grants-2010_04 |
|---|
| ORD ID | ord-7f10b811aa024744bf8ca76282d17f55 |
|---|
| 出典メモ | uspto-grants-2010_04 |
|---|