化工社化工社 化学情報印刷レポート · 研究参考用
Iodoethane → 1-Ethoxy-5-fluoro-4-methyl-2-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Fluoro-4-methyl-2-nitrophenol | HCID 12782411 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Ethoxy-5-fluoro-4-methyl-2-nitrobenzene | HCID 59452883 | 60.6% |
反応手順
4-Methyl-5-fluoro-2-nitrophenol (11.1 g, 65.0 mmol) and iodoethane (12.2 g, 78.0 mmol) were dissolved in 100 mL of DMSO with stirring. K2CO3 (13.5 g, 97.5 mmol) was added. The reaction was stirred for 3 h and then diluted with DCM and filtered. The filtrate was poured into H2O and extracted with DCM. The combined organic layers were dried over MgSO4, filtered, and concentrated in vacuo to provide the title compound of step A (8.0 g, 39.4 mmol) as a pale yellow crystalline solid. 1H NMR (400 MHz, CDCl3) δ 7.76 (d, J=8.1 Hz, 1H), 6.70 (d, J=11.0 Hz, 1H), 4.10 (q, J=7.0 Hz, 2H), 2.22 (s, 3H), 1.45 (t, J=7.0 Hz, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08093239B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-f8596cf6d2564e7abe2e4f04878f3b32 |
| 出典メモ | uspto-grants-2012_01 |