Hydrochloric Acid → HCID 69130760, compound

HRID 131076Notes

Reaction equation

HRID 131076 reaction equation
[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]

Participants

4

Procedure

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).

Workup

  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

Sources & evidence

ORD record
ord-ab1032e0e19f4f00a684b1952f086dab
Source dataset
uspto-grants-2008_06
Patent number
US07384789B2

Reaction notes

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