化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → Methyl 4'-hydroxy(1,1'-biphenyl)-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4'-Hydroxy-4-biphenylcarboxylic acid | HCID 301556 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 4'-hydroxy(1,1'-biphenyl)-4-carboxylate | HCID 1490289 | 86% |
反応手順
Concentrated sulfuric acid (approximately 4 ml) was carefully added to a solution of 4'-hydroxy-4-biphenylcarboxylic acid (Aldrich) (8.20 g, 38.3 mmol) in 1 liter of methanol. The reaction mixture was refluxed for three days and the solvent was evaporated. The resulting solid was filtered, washed with water, and recrystallized as follows. The crude solid was dissolved in a minimum amount of hot THF, and approximately three equivalents of methanol was added to the solution. The solution was brought to a boil, and water was added with vigorous stirring until the solution remained cloudy. After cooling, the tan precipitate was filtered, washed with cold ethanol, and air dried to yield 7.57 g (86%) of a tan solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06139771 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-53bce1ae08354a239459042c108dfb00 |
| 出典メモ | uspto-grants-2000_10 |