化工社化工社 化学情報印刷レポート · 研究参考用
2-Methyl-9-fluorenecarboxylic acid → 2-Methyl-9-fluorenemethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methyl-9-fluorenecarboxylic acid | HCID 19978418 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Methyl-9-fluorenemethanol | HCID 15045058 | 80.7% |
反応手順
A solution of 2-methyl-9-fluorenecarboxylic acid (6 g, 26.8 mmol) in 300 mL of THF at 0° C. was charged with IM THF solution of BH3-THF complex (53.5 mL, 53.5 mmol). The reaction mixture was stirred overnight then quenched with 30 mL of 10% acetic acid in methanol and diluted with 300 mL of water. The layers were separated, the aqueous phase was extracted with ethyl acetate (3×50 mL), the combined extracts were dried over magnesium sulfate and evaporated to give colorless oil. Crystallization was accomplished upon treatment of the oil with 200 mL of hexane. Recrystallization from ethanol:water 4:1 afforded 4.55 g (80.6%) of 2-methyl-9-fluorenemethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05079260 |
| 出典データセット | uspto-grants-1992_01 |
| ORD ID | ord-0e55f2c32a4840bb82489d2f96734c46 |
| 出典メモ | uspto-grants-1992_01 |