N-bromobutanimide → 3-(Bromomethyl)-2,5-dichlorothiophene
反応式
[Cl:1][C:2]1[S:3][C:4]([Cl:8])=[CH:5][C:6]=1[CH3:7].[Br:9]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:9][CH2:7][C:6]1[CH:5]=[C:4]([Cl:8])[S:3][C:2]=1[Cl:1]参加物
5
実験手順
To a stirred solution of 2,5-dichloro-3-methylthiophene (25.8 g, 154 mmol) in carbon tetrachloride (47 mL) was added N-bromosuccinimide (27.5 g, 154 mmol) and benzoyl peroxide (310 mg, 1.28 mmol). The mixture was heated at reflux temperature for 8 hours. After cooling, the insolubles were filtered off. The filtrate was washed with aqueous sodium sulfite solution, dried over MgSO4, and concentrated in vacuo. The residue was fractionally distilled under reduced pressure (bp 80° C., 0.5 mmHg) to give the subtitle compound (34.5 g, 91% yield).
後処理
- temperatureThe mixture was heated
- temperatureat reflux temperature for 8 hours
- temperatureAfter cooling
- filtrationthe insolubles were filtered off
- washThe filtrate was washed with aqueous sodium sulfite solution
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- distillationThe residue was fractionally distilled under reduced pressure (bp 80° C., 0.5 mmHg)
出典と根拠
- ORDレコード
- ord-1af66f65e8ce4500976f36b61b2ee0ae
- 出典データセット
- uspto-grants-2004_02
- 特許番号
- US06696470B2
反応ノート
読み込み中…