Hydrochloric Acid → HCID 69130760、化合物

HRID 131076ノート

反応式

HRID 131076 の反応式
[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

  1. dissolutionwere dissolved), the solution
  2. temperaturewas cooled to 4° C
  3. customThe product was collected as a white precipitate
  4. 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

読み込み中…