化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 2,4-Diisopropyldibenzo[b,d]furan-1-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 3,4-Di(prop-1-en-2-yl)dibenzo[b,d]furan-1-amine | HCID 118426694 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 生成物 | 2,4-Diisopropyldibenzo[b,d]furan-1-amine | HCID 58401076 | 68% |
反応手順
3,4-di(prop-1-en-2-yl)dibenzo[b,d]furan-1-amine (4.8 g, 18.2 mmol), and 5% Pt/C (0.48 g) and 10% Pd/C (0.48 g) were added to a mixture of ethanol (90 mL) and acetic acid (10 mL). Reaction mixture was hydrogenated overnight at 50 psi. Reaction mixture was filtered through a Celite pad and most of the organic solvent was evaporated under vacuum. Crude product was dissolved in ethylacetate and partitioned between 1N NaOH and ethylacetate to get rid of any acetic acid. Organic layer was dried over anhydrous Na2SO4, evaporated under vacuum and purified by flash chromatography over silica gel with 40% DCM/hexanes. Target compound (3.3 g, 68%) was isolated as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09156870B2 |
| 出典データセット | uspto-grants-2015_10 |
| ORD ID | ord-079e39cb1c954671a313f07472917fda |
| 出典メモ | uspto-grants-2015_10 |