化工社化工社 化学情報印刷レポート · 研究参考用
Water → Tropenol 9-hydroxyfluorene-9-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl 9-hydroxy-9H-fluorene-9-carboxylate | HCID 267210 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Tropenol | HCID 53629842 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Tropenol 9-hydroxyfluorene-9-carboxylate | HCID 86593872 | — |
反応手順
13.4 g (0.056 mol) of methyl ester 3a, 11.65 g (0.084 mol) of tropenol, and 0.3 g of sodium are heated as a melt at 75 mbar for 4 hours over a bath of boiling water with occasional agitation. After cooling, the sodium residues are dissolved with acetonitrile, the solution is evaporated to dryness, and the residue is extracted with dichloromethane/water. The organic phase is washed with water, dried over magnesium sulfate (MgSO4), and the solvent is distilled off. The product is purified by recrystallization from diethyl ether. Yield: 11.40 g of white crystals (29% 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-b304d4c32fef404f97a5da0ed3d58746 |
| 出典メモ | uspto-grants-2008_09 |