Carbon tetrabromide → 2-Methoxyphenethyl bromide
反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[CH2:5][CH2:6]O.C(Br)(Br)(Br)[Br:13].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[CH2:5][CH2:6][Br:13]参加物
5
反応条件
- 温度
- 0 °C
実験手順
A mixture of 2-methoxyphenethyl alcohol (500 mg) and carbon tetrabromide (1.53 g) in anhydrous dichloromethane (10 mL) was stirred at 0° C. under a nitrogen atmosphere. After adding triphenylphosphine (1.03 g) portionwise, the reaction mixture was stirred for an hour under the same condition. The reaction mixture was evaporated in vacuo and the residue was subjected to a silica gel column chromatography eluting with n-hexane only and then a mixture of n-hexane and ethyl acetate (40:1 to 20:1) to give 2-methoxyphenethyl bromide (661 mg) as an oil.
後処理
- stirringthe reaction mixture was stirred for an hour under the same condition
- customThe reaction mixture was evaporated in vacuo
- washeluting with n-hexane only
- additiona mixture of n-hexane and ethyl acetate (40:1 to 20:1)
出典と根拠
- ORDレコード
- ord-3c6b7c184f2446658afad0c863a096b9
- 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…