(Chlorothio)formyl chloride → 5-(4-Chloro-2-methoxyphenyl)-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])=[C:4]([O:11][CH3:12])[CH:3]=1.Cl[C:14]([S:16]Cl)=[O:15]>O1CCCC1>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]2[O:7][C:14](=[O:15])[S:16][N:8]=2)=[C:4]([O:11][CH3:12])[CH:3]=1参加物
4
実験手順
In tetrahydrofuran (100 ml), 4-chloro-2-methoxybenzamide (5.67 g, 30.5 mmol) prepared in the Step 7-1-1 and chlorocarbonylsulfenyl chloride (4.40 g, 33.6 mmol) were suspended, and the mixture was heated under reflux for 1.5 hours. After being allowed to cool, the mixture was subjected to extraction with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and then concentrated. The concentrate was purified by silica gel column chromatography (n-hexane:ethyl acetate=7:1) to give the title compound (5.33 g, 71%).
後処理
- temperaturethe mixture was heated
- temperatureunder reflux for 1.5 hours
- temperatureto cool
- extractionthe mixture was subjected to extraction with ethyl acetate
- dry with materialthe extract was dried over anhydrous magnesium sulfate
- concentrationconcentrated
- customThe concentrate was purified by silica gel column chromatography (n-hexane:ethyl acetate=7:1)
出典と根拠
- ORDレコード
- ord-bbbecceb172e405d9d3af1c5778f1aaa
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09200008B2
反応ノート
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