Hydrochloric Acid → HCID 69130760、化合物
反応式
[CH3:1][O:2][C:3]1[C:8]([N+:9]([O-])=O)=[CH:7][C:6]([CH3:12])=[CH:5][C:4]=1[N+:13]([O-])=O.[Sn].[ClH:17]>>[ClH:17].[NH2:13][C:4]1[CH:5]=[C:6]([CH3:12])[CH:7]=[C:8]([NH2:9])[C:3]=1[O:2][CH3:1]参加物
4
実験手順
2-Methoxy-5-methyl-1,3-dinitrobenzene (0.050 g, 0.236 mmol) was suspended in conc. Hydrochloric acid (1.2 mL). Tin granules (0.118 g, 0.995 mmol) were added slowly to the mixture with stirring at room temperature. After 2 hours, the solution turned white (all the tin granules were dissolved), the solution was cooled to 4° C. The product was collected as a white precipitate and recrystallized from hot water-concentrated hydrochloric acid. Yield=0.037 g (70%) from 0.050 g 2-Methoxy-5-methyl-1,3-dinitrobenzene. White flakes; mp 226° C. (dec); 1H NMR (DMSO) δ: 6.57 (s, 2H), 3.91 (s, broad, 6H), 3.72 (s, 3H), 2.17 (s, 3H).
後処理
- dissolutionwere dissolved), the solution
- temperaturewas cooled to 4° C
- customThe product was collected as a white precipitate
- customrecrystallized from hot water-concentrated hydrochloric acid
出典と根拠
- ORDレコード
- ord-ab1032e0e19f4f00a684b1952f086dab
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07384789B2
反応ノート
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