化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → 1-[2,5-Bis(2,2,2-trifluoroethoxy)phenyl]-3-(4-methylphenyl)-2-propen-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 4-Methylbenzaldehyde | HCID 7725 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(2,5-Bis(2,2,2-trifluoroethoxy)phenyl)ethan-1-one | HCID 2736073 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-[2,5-Bis(2,2,2-trifluoroethoxy)phenyl]-3-(4-methylphenyl)-2-propen-1-one | HCID 90729888 | — |
反応手順
The title compound was prepared by heating a mixture of 2,5-bis(2,2,2-trifluoroethoxy)acetophenone (200 mg, 0.633 mmol), p-tolualdehyde (75 ul, 0.633 mmol), methanol (5 ml) and NaOH (200 ul, 10M) for 24 h. The mixture was cooled to room temperature, diluted with ethyl acetate (100 ml), wash with water and saturated aqueous NaCl, dried over anhydrous sodium sulfate and then concentrated in vacuo. The residue was purified by column chromatography using hexane:ethyl acetate (4:1) to give a yellow solid (32 mg, 12.2%). 1H NMR (CDCl3): 7.67 (d, J=15.6 Hz, 1H), 7.50 (d, J=8.4 Hz, 2H), 7.40 (d, J=15.6 Hz, 1H), 7.28 (d, J=3.3 Hz, 1H), 7.22 (d, J=8.1 Hz, 2H), 7.12 (dd, J=3.3, 9.3 Hz, 1H), 6.96 (d, J=8.7 Hz, 1H), 4.44-4.33 (m, 4H), 2.39 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07256219B2 |
| 出典データセット | uspto-grants-2007_08 |
| ORD ID | ord-90207729a5b2405e8a0e912ea96eef0c |
| 出典メモ | uspto-grants-2007_08 |