関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitroethane | HCID 6587 | — |
| 反応物 | Cyclohexylamine | HCID 7965 | — |
| 反応物 | 2,5-Difluorobenzaldehyde | HCID 137663 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-(2,5-Difluorophenyl)-2-nitropropene | HCID 66690528 | 81.3% |
反応手順
A mixture of 2,5-difluorobenzaldehyde (25.0 g, 0.176 mol), nitroethane (26.41 g, 0.352 mol) and cyclohexylamine (17.45 g, 0.176 mol) in 150 mL of acetic acid was stirred at 80° C. overnight. After cooling to rt the solvent was evaporated, the residue was purified by column chromatography (silica-gel, CH2Cl2/acetone=19/1 v/v) to give a yellow solid product, 28.5 g, 81.3% yield. MS: 197.6 [M−H]−. 1H NMR (DMSO-d6, 500 MHz): δ 7.94 (s, 1H), 7.46-7.43 (m, 1H), 7.41-7.35 (m, 2H), 2.31 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08822500B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-1c9a8319490d48369f38e5846bbd8c50 |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|
