Phosphorus tribromide → 5-(Bromomethyl)-2-methoxybenzonitrile
反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH2:6]O)#[N:2].P(Br)(Br)[Br:14]>ClCCl>[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH2:6][Br:14])#[N:2]参加物
4
反応条件
- 温度
- 0 °C
実験手順
To a solution of 3-cyano-4-methoxybenzyl alcohol (500 mg) in dichloromethane (5 mL) was added phosphorus tribromide (0.146 mL) under ice-water cooling. The mixture was stirred at 0° C. for 3 hours and partitioned between chloroform and water. The separated organic layer was washed successively with water, an aqueous saturated sodium bicarbonate solution and brine. The organic layer was dried over magnesium sulfate and evaporated in vacuo. The residual solid was triturated with diisopropyl ether to give 3-cyano-4-methoxybenzyl bromide as an off-white solid (456.3 mg).
後処理
- custompartitioned between chloroform and water
- washThe separated organic layer was washed successively with water
- dry with materialThe organic layer was dried over magnesium sulfate
- customevaporated in vacuo
- customThe residual solid was triturated with diisopropyl ether
出典と根拠
- ORDレコード
- ord-e86e137fd44248c0a693a50727711c04
- 出典データセット
- uspto-grants-2003_06
- 特許番号
- US06582351B1
反応ノート
読み込み中…