Carbon tetrabromide → HCID 18331400、化合物
反応式
[CH2:1]([O:3][C:4]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6]O)[CH3:2].C(Br)(Br)(Br)[Br:16].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[CH2:1]([O:3][C:4]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6][Br:16])[CH3:2]参加物
5
実験手順
To a mixture of the compound (3.13 g) obtained in Example 417b, carbon tetrabromide (5.26 g) and methylene chloride (100 ml), triphenylphosphine (4.16 g) was added under ice cooling. The reaction mixture was stirred under ice cooling for 30 min and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate: n-hexane=1:9) to give 3.59 g of the titled compound (yield, 87%).
後処理
- additionwas added under ice cooling
- concentrationconcentrated under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate: n-hexane=1:9)
出典と根拠
- ORDレコード
- ord-b2416b45a35548c5bfc7da59f79fa1fd
- 出典データセット
- uspto-grants-2001_12
- 特許番号
- US06331553B1
反応ノート
読み込み中…