関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | 1-Bromo-2-(bromomethyl)-3-nitrobenzene | HCID 15063170 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Bromo-6-nitrobenzyl Acetate | HCID 58824122 | — |
反応手順
To a solution of 1-bromo-2-bromomethyl-3-nitro-benzene (3.39 g, 11.53 mmol) in DMF (50 nml) was added KOAc (7.6 g, 77.4 mmol). The reaction was heated at 70° C. for an hour. After cooling to room temperature, the mixture was partitioned between water and ethyl acetate. The organic layer was washed with water and brine, and dried over MgSO4 Acetic acid 2-bromo-6-nitro-benzyl ester (3.1 g) was obtained as a brown oil after concentration under vacuum (˜100%). 1H NMR (CDCl3, 300 MHz) δ: 2.06(s, 3H), 5.46 (s, 2H), 7.377(t, J=8.1 Hz), 7.778(dd, J=1.23 Hz, 8.14 Hz), 7.856(dd, J=1.23 Hz, 8.07 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07196087B2 |
|---|
| 出典データセット | uspto-grants-2007_03 |
|---|
| ORD ID | ord-2b245187379b4f5c91e535abb54e0584 |
|---|
| 出典メモ | uspto-grants-2007_03 |
|---|