Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine-2-sulfonic acid allyl-(2-methyl-pent-4enyl)-amide → 3-Methyl-1-(pyridine-2-sulfonyl)-2,3,4,7-tetrahydro-1H-azepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine-2-sulfonic acid allyl-(2-methyl-pent-4enyl)-amide | HCID 11565389 | — |
| 촉매 | HCID 178479819 | HCID 178479819 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Methyl-1-(pyridine-2-sulfonyl)-2,3,4,7-tetrahydro-1H-azepine | HCID 11630223 | 83% |
반응 단계
Pyridine-2-sulfonic acid allyl-(2-methyl-pent-4-enyl)-amide (1.2 g, 4.3 mmol) was diluted in CH2Cl2 (100 ml). After carefully degass by Ar, Grubbs catalyst (0.35 g, 0.43 mmol) was added under Ar protection. The mixture was then refluxed for 2 h before the reaction mixture was concentrated by rotary evaporation. The product was purified by column chromatography (5%-20% EtOAc/hexanes) to give the title compound (0.9 g, 83% yield): MS (M+H+):253.2; 1H-NMR (400 Hz, CDCl3): d=8.70(d, 1H), 8.0-7.75(m, 2H), 7.5 (m, 1H) 5.79-5.60(m, 2H), 4.00(d, 2H), 3.65(dd, 1H), 3.22(dd, 1H), 2.30-2.05(m, 3H), 0.96(d, 3H)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07563784B2 |
| 출처 데이터셋 | uspto-grants-2009_07 |
| ORD ID | ord-a3ea2d4def5041b6a36644d1314d6122 |
| 출처 메모 | uspto-grants-2009_07 |