Sulfamide → Sulfamic acid chroman-2-ylmethyl amine
反応式
[O:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH:2]1[CH2:11][NH2:12].[S:13](N)([NH2:16])(=[O:15])=[O:14]>O1CCOCC1>[O:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH:2]1[CH2:11][NH:12][S:13]([NH2:16])(=[O:15])=[O:14]参加物
4
実験手順
The oily amine (1.63 g, 10 mmol) and sulfamide (1.92 g, 20 mmol) were combined in dioxane (50 mL) and brought to reflux for 2 h. The solution was cooled and evaporated in vacuo to yield an oil, which was purified via column chromatography (DCM:Methanol 10:1) to yield a white solid. The solid was recrystallized from ethyl acetate/hexane to yield chroman-2-ylmethylsulfamide as a white solid.
後処理
- temperatureto reflux for 2 h
- temperatureThe solution was cooled
- customevaporated in vacuo
- customto yield an oil, which
- customwas purified via column chromatography (DCM:Methanol 10:1)
- customto yield a white solid
- customThe solid was recrystallized from ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-7d23da7f06bb435c8177cfaf5f03ed59
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08716231B2
反応ノート
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