関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | 2-Chloro-4-(hydroxymethyl)-3-methylbenzonitrile | HCID 68577571 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(Bromomethyl)-2-chloro-3-methylbenzonitrile | HCID 68577413 | 28.3% |
反応手順
To a solution of compound 7B (700 mg, 3.9 mmol) in CH2Cl2 (15 mL) was added PBr3 (5.8 mL, 5.8 mmol, 1N in CH2Cl2) at −15° C., and stirred at −15° C. for 3 hr. The reaction was slowly quenched with saturated NaHCO3 solution at −15° C. The organic layer was separated, dried over MgSO4, and concentrated. Purification by silica gel chromatography (0-10% EtOAc in hexanes) provide the title compound (270 mg) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07732480B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-a53eda7a21c6493b8351a35a680eae0b |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|
