Stannous chloride dihydrate → 6-chloro-7-methyl-3,4-dihydroquinoxalin-2(1H)-one
反応式
[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]2参加物
4
実験手順
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 and 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 (DMSO-d6): δ2.093 (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).
後処理
- filtrationthe precipitated solid was filtered
- washwashed with ethanol (4.0 mL)
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-320d60f9a6d0463695a7580e7e302485
- 出典データセット
- uspto-grants-1997_05
- 特許番号
- US05631373
反応ノート
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