N-bromobutanimide → Dimethyl bromomethylfumarate
反応式
[CH3:1][O:2][C:3](=[O:11])/[C:4](/[CH3:10])=[CH:5]\[C:6]([O:8][CH3:9])=[O:7].[Br:12]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.N(C(C)(C)C#N)=NC(C)(C)C#N>[CH3:1][O:2][C:3](=[O:11])/[C:4](/[CH2:10][Br:12])=[CH:5]/[C:6]([O:8][CH3:9])=[O:7]参加物
5
実験手順
To a solution of (Z)-2-methyl-2-butenedioic acid dimethyl ester (15.3 g) in carbon tetrachloride (300 ml) were added N-bromosuccinimide (25.8 g) and 2,2′-azobis(isobutyronitrile) (319 mg), and the mixture was stirred for 36 hours at reflux. After cooling the mixture to room temperature, the insoluble substance was filtered off, and the filtrate was concentrated. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/0 to 18/1) to give the titled compound (19.6 g).
後処理
- temperatureat reflux
- filtrationthe insoluble substance was filtered off
- concentrationthe filtrate was concentrated
- customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/0 to 18/1)
出典と根拠
- ORDレコード
- ord-9b68949a788e4e38b52d66d0a597807e
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846746B2
反応ノート
読み込み中…