反応式
[CH3:1][O:2][C:3](=[O:22])[CH2:4][CH2:5][C:6](=[O:21])[CH2:7][NH:8][C:9]([C:11]1[CH:12]=[C:13]([CH:18]=[CH:19][CH:20]=1)[C:14]([O:16][CH3:17])=[O:15])=O.[OH-].COC(NS([N+](CC)(CC)CC)(=O)=O)=O>O1CCCC1>[CH3:1][O:2][C:3](=[O:22])[CH2:4][CH2:5][C:6]1[O:21][C:9]([C:11]2[CH:12]=[C:13]([CH:18]=[CH:19][CH:20]=2)[C:14]([O:16][CH3:17])=[O:15])=[N:8][CH:7]=1参加物
4
実験手順
Methyl 3-{[(5-methoxy-2,5-dioxopentyl)amino]carbonyl}benzoate (520 mg, 1.7 mmol) is dissolved in anhydrous tetrahydrofuran (4 mL), and (methoxycarbonylsulfamoyl)triethylammonium hydroxide, inner salt (810 mg, 3.4 mmol). The reaction is microwaved (100 W. 2 min) in a sealed vessel, cooled, filtered, and concentrated under reduced pressure. Purification by flash chromatography (silica gel, 40% ethyl acetate/hexanes) gives the title compound. ESI MS m/z 290.1 [M+H]+.
後処理
- customThe reaction is microwaved (100 W. 2 min) in a sealed vessel
- temperaturecooled
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customPurification by flash chromatography (silica gel, 40% ethyl acetate/hexanes)
出典と根拠
- ORDレコード
- ord-907bd4bbca564b108daa5d4bf0fa9f69
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07176242B2
関連ノート
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