化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl Acetate → 1-(2-Amino-4-(benzyloxy)-5-methoxyphenyl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 反応物 | 1-(4-(Benzyloxy)-5-methoxy-2-nitrophenyl)ethanone | HCID 53486760 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(2-Amino-4-(benzyloxy)-5-methoxyphenyl)ethanone | HCID 22667147 | 86% |
反応手順
A mixture of 1-(4-(benzyloxy)-5-methoxy-2-nitrophenyl)ethanone (3.6 g, 12 mmol), iron powder (4.5 g) and ammonium formate (5.5 g) in toluene (50 mL) and water (50 mL) was heated at reflux temp. for 2 days with stirring. To this mixture was added EtOAc (100 mL), stirred for 20 minutes, the solid was filtered through a celite bed and washed with EtOAc (150 mL). The EtOAc layer was separated from the filtrate solution, washed with water (2×100 mL), dried over MgSO4 and concentrated in vacuo to afford the product (2.80 g, 86%) as a beige-colored solid. 1H NMR (CDCl3) δ 7.41-7.30 (m, 5H), 7.13 (s, 1H), 6.15 (br s, 2H), 6.10 (s, 1H), 5.13 (s, 2H), 3.84 (s, 3H), 2.51 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732613B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-b943a218c56d48dc861cd550476831fc |
| 出典メモ | uspto-grants-2010_06 |