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Phosphorus tribromide → 2-Bromomethyl-1,3-dichloro-4-methoxy-benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | (2,6-Dichloro-3-methoxyphenyl)methanol | HCID 21980844 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Bromomethyl-1,3-dichloro-4-methoxy-benzene | HCID 59299515 | 112.7% |
反応手順
Dissolve (2,6-dichloro-3-methoxy-phenyl)-methanol (9.43 g, 45.5 mmol) in methylene chloride (180 ml) cool to 0° and add phosphorus tribromide (1.0M, 23 ml, 23 mmol) dropwise. Stir for 10 minutes at 0°, dilute with methylene chloride, quench with saturated aqueous sodium bicarbonate, separate layers, wash organic with water, brine dry over sodium sulfate, filter and concentrate to yield 7 g (57%) of the title compound: NMR (CDCl3) δ 7.28 (d, 1H), 6.85 (d, 1H), 4.77 (s, 2H), 3.90 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07713979B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-cbef151c5f774ed692a952346e03f5d5 |
| 出典メモ | uspto-grants-2010_05 |