Chlorosulfamic acid → 2-Sulfamoylaminocyclopent-1-enecarbonitrile
反応式
[NH2:1][C:2]1[CH2:6][CH2:5][CH2:4][C:3]=1[C:7]#[N:8].[S:9](Cl)(=[O:12])(=[O:11])[NH2:10]>CC(N(C)C)=O.CCOC(C)=O>[S:9]([NH:1][C:2]1[CH2:6][CH2:5][CH2:4][C:3]=1[C:7]#[N:8])(=[O:12])(=[O:11])[NH2:10]参加物
5
実験手順
To a solution of 2-aminocyclopent-1-enecarbonitrile (440 mg, 4.07 mmol) in 10 mL of DMA was added sulfamoyl chloride (941.3 mg, 8.15 mmol), and the resultant mixture was stirred at room temperature under nitrogen for 2 h. Then it was diluted with EtOAc, the organic layer was washed with brine and dried down under vacuum, and the residue was purified by chromatography on silica gel eluting with EtOAc/Hexane to give the title compound. 1H NMR (400 MHz, CDCl3) δ 2.04-1.97 (m, 2H), 2.61-2.57 (m, 2H), 2.9-2.86 (m, 2H), 5.66 (s, 2H), 8.04 (s, 1H).
後処理
- washthe organic layer was washed with brine
- customdried down under vacuum
- customthe residue was purified by chromatography on silica gel eluting with EtOAc/Hexane
出典と根拠
- ORDレコード
- ord-4ba72409f52b490d85f07decf4d090eb
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181276B2
反応ノート
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