Carbon tetrabromide → 4-Bromo-1-(bromomethyl)-2-methylbenzene
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]O)=[C:4]([CH3:10])[CH:3]=1.C(Br)(Br)(Br)[Br:12].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][Br:12])=[C:4]([CH3:10])[CH:3]=1参加物
5
実験手順
To a stirred solution of (4-Bromo-2-methyl-phenyl)-methanol (as obtained in preparation 25) (4.58 g, 22.8 mmol) in CH2Cl2 (50 ml) is added, under Argon and at RT, carbon tetrabromide (9.27 g, 27.4 mmol) followed by triphenylphosphine (7.25 g, 27.4 mmol). The mixture is stirred overnight and then concentrated in vacuo. The crude residue is then purified by chromatography (silicagel, hexane:EtOAc 25:1) to afford the title compound as a clear oil.
後処理
- concentrationconcentrated in vacuo
- customThe crude residue is then purified by chromatography (silicagel, hexane:EtOAc 25:1)
出典と根拠
- ORDレコード
- ord-8425ad05259042d4b6c8c395a867b1f5
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08193189B2
反応ノート
読み込み中…