4-Chlorobenzamide → 5-(4-Chlorophenyl)-1,3,4-oxathiazol-2-one
反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][CH:3]=1.Cl[C:12]([S:14]Cl)=[O:13]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]2[O:7][C:12](=[O:13])[S:14][N:8]=2)=[CH:4][CH:3]=1参加物
4
反応条件
- 温度
- 80 °C
実験手順
To a solution of 4-chlorobenzamide (1.0 g, 6.42 mmol) in toluene (25 ml) was added chlorocarbonylsulfenyl chloride (1.0 ml, 12.85 mmol). The resulting reaction mixture was refluxed at 80° C. for 3 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added diethyl ether and washed twice with water, twice with 5% NaHCO3, again with water, and was dried (Na2SO4), concentrated under vacuum to give the product (crude yield 1.37 g, 100%) that was carried forward to the next step without further purification.
後処理
- customThe resulting reaction mixture
- customAfter the completion of the reaction (TLC monitoring)
- concentrationthe mixture was concentrated
- additionadded diethyl ether
- washwashed twice with water, twice with 5% NaHCO3, again with water
- dry with materialwas dried (Na2SO4)
- concentrationconcentrated under vacuum
- customto give the product (crude yield 1.37 g, 100%) that
- customwas carried forward to the next step without further purification
出典と根拠
- ORDレコード
- ord-d8fbdce758a14dc59101fae7679a5723
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08415383B2
反応ノート
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