Stannous chloride dihydrate → 6-chloro-7-methyl-3,4-dihydroquinoxalin-2(1H)-one
반응식
[Cl:1][C:2]1[C:3]([CH3:16])=[CH:4][C:5]([N+:13]([O-])=O)=[C:6]([NH:8][CH2:9][C:10](O)=[O:11])[CH:7]=1.O.O.[Sn](Cl)Cl>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]2[C:5](=[CH:4][C:3]=1[CH3:16])[NH:13][C:10](=[O:11])[CH2:9][NH:8]2참가 물질
4
실험 절차
A solution of N-(5′-chloro-4′-methyl-2′-nitrophenyl)glycine (1.000 g, 4.088 mmol, as prepared above) and tin (II) chloride dihydrate (2.767 g, 12.26 mmol, Aldrich, used as received) in ethanol (20.0 mL) was refluxed for 30 min. It was then cooled to room temperature ad the precipitated solid was filtered, washed with ethanol (4.0 mL), and dried under vacuum to yield 0.251 g (31%) of the title compound as a yellow powder; 1H NMR (DMSOd6): δ 2.093 (s, 3H), 3.657 (d, 2H, J=1.5 Hz), 5.984 (s, 1H), 6.583 (s, 1H), 6.632 (s, 1H), 10.253 (s, 1H).
후처리
- filtrationwas filtered
- washwashed with ethanol (4.0 mL)
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-5d73c08ffd2b4730be7d25b437e83ff9
- 출처 데이터셋
- uspto-grants-2001_06
- 특허 번호
- US06251903B1
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