化工社化工社 化学情報印刷レポート · 研究参考用
Dimethyl Sulfate → Benzene, 1,3-dibromo-2-methoxy-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,6-Dibromophenol | HCID 11847 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Benzene, 1,3-dibromo-2-methoxy- | HCID 181584 | 96% |
反応手順
A mixture of 2,6-dibromophenol (25 g, 0.099 mol), powder potassium carbonate (28 g, 0.2 mol, 2 equiv) and dimethyl sulfate (12.6 g, 0.099 mol) in acetonitrile (400 mL) was kept at reflux with good stirring for 4 hr. After cooling, the solids were removed by filtration and the solvent was removed in a rotary evaporator. The residue was taken in 2:1 heptane/ethyl acetate mixture (800 mL) and washed with water (2×400 mL). The organic layer was dried over sodium sulfate, filtered and the solvent was removed in a rotary evaporator, leaving almost pure 1 (15.5 g, 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08557936B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-99facb1a8b3543a985521627d332adbc |
| 出典メモ | uspto-grants-2013_10 |