化工社化工社 化学情報印刷レポート · 研究参考用
Sulfuric Acid → Methyl 9-hydroxy-9H-fluorene-9-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Flurenol | HCID 10087 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 9-hydroxy-9H-fluorene-9-carboxylate | HCID 267210 | — |
反応手順
50.4 g (0.223 mol) of 9-hydroxy-9-fluorenecarboxylic acid are dissolved in 500 mL of methanol, combined with 5 mL (0.089 mol) of concentrated sulfuric acid and refluxed for 1 hour. After cooling, 100 mL of sodium hydrogen carbonate solution (about pH 8) are added and the methanol is largely evaporated down. The mixture is extracted with dichloromethane and water, the organic phase is dried and evaporated to dryness. The product is purified by recrystallization from ethyl acetate. Yield: 50.0 g of white crystals (93% of theoretical yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429600B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-4574abed5e3f4c42926a5f9dfb8c0947 |
| 出典メモ | uspto-grants-2008_09 |