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Methanol → 1-(Bromomethyl)-2-methoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | 2-Methoxybenzyl alcohol | HCID 69154 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(Bromomethyl)-2-methoxybenzene | HCID 40308 | 137.2% |
反応手順
To a solution of 1-hydroxymethyl-2-methoxy-benzene (28.7 g, 0.207 mol) in CH2Cl2 (574 mL) at 0° C. under nitrogen was added slowly PBr3 (13.66 mL, 0.145 mol). After stirring for an additional 1.5 hours, MeOH (13.66 mL) was added and stirred for 5 minutes. To this mixture was added dropwise 10% Na2CO3 (2 mL) solution and stirred for 5 minutes. The mixture was then washed with 10% Na2CO3 (50 mL, 2×) and brine (100 mL). It was dried over MgSO4, and filtered. The filtrate was removed under vacuum to give an oil (40 g) of 1-bromomethyl-2-methoxy-benzene. This material was used without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05892039 |
| 出典データセット | uspto-grants-1999_04 |
| ORD ID | ord-f35e4f153c7a4acfb995cadb074ea647 |
| 出典メモ | uspto-grants-1999_04 |