Sulfuric Acid → 2,6-Dichloro-4-methylbenzamide
反応式
[Cl:1][C:2]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([Cl:11])[C:3]=1[C:4]#[N:5].S(=O)(=O)(O)[OH:13]>>[Cl:1][C:2]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([Cl:11])[C:3]=1[C:4]([NH2:5])=[O:13]参加物
3
実験手順
To stirred, cooled concentrated sulfuric acid (40 ml) was added in portions 2,6-dichloro-4-methylbenzonitrile (13.2 g, 71.0 mmol). The mixture was heated on a steam bath for 3 hours with occasional shaking, cooled, poured into ice-water, and extracted twice with dichloromethane. The combined extracts were washed with brine, dried over anhydrous magnesium sulfate, and evaporated under vacuum. The residue was chromatographed on a column of silica gel (390 g) eluted with 4:1 (v/v) dichloromethane-diethyl ether to provide 8.6 g (59%) of 2,6-dichloro-4-methylbenzamide, m.p. 101°-107° C.
後処理
- temperatureThe mixture was heated on a steam bath for 3 hours with occasional shaking
- temperaturecooled
- extractionextracted twice with dichloromethane
- washThe combined extracts were washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated under vacuum
- customThe residue was chromatographed on a column of silica gel (390 g)
- washeluted with 4:1 (v/v) dichloromethane-diethyl ether
出典と根拠
- ORDレコード
- ord-86059a1560274fa6b6651c7a841f8c25
- 出典データセット
- uspto-grants-1986_05
- 特許番号
- US04590201
反応ノート
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