関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 1,3-Dibromo-2-(bromomethyl)benzene | HCID 13381015 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,6-Dibromobenzyl acetate | HCID 59216413 | 95% |
反応手順
A mixture of 1,3-dibromo-2-(bromomethyl)benzene (27.6 g, 84 mmol), NaOAc (35.5 g, 5 eq.) and dimethylformamide (DMF) (150 mL) was stirred at 100° C. (hot oil bath temperature) for 1.75 h, allowed to cool, and then partitioned between heptane (500 mL) and water (200 mL). After removing the organic layer, the aqueous layer was extracted with heptane (200 mL). The combined organics were washed with H2O (2×300 mL), dried (Na2SO4), filtered, and evaporated to give 24.57 g (yield of 95%) of title product as a colorless oil. This oil contained 13% unreacted starting material but was successfully used without further purification. 1H NMR (300 MHz, CDCl3) δ 2.10 (s, 3H), 5.41 (s, 2H), 7.08 (t, 1H), 7.58 (d, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08759340B2 |
|---|
| 出典データセット | uspto-grants-2014_06 |
|---|
| ORD ID | ord-be467ddb4b66466d8687c9f381268551 |
|---|
| 出典メモ | uspto-grants-2014_06 |
|---|