Chlorosulfamic acid → 2-Sulfamoylaminocyclopent-1-enecarbonitrile
반응식
[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]참가 물질
5
실험 절차
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).
후처리
- washthe organic layer was washed with brine
- customdried down under vacuum
- customthe residue was purified by chromatography on silica gel eluting with EtOAc/Hexane
출처 및 근거
- ORD 기록
- ord-4ba72409f52b490d85f07decf4d090eb
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09181276B2
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