Hydrochloric Acid → HCID 20389417, compound

HRID 1348500Notes

Reaction equation

HRID 1348500 reaction equation
[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[CH:7]=[C:6]([CH3:13])[C:5]=1[O:14][CH3:15])([O-])=O.C(O)C.[H][H].[ClH:21]>[Pd].O>[ClH:21].[ClH:21].[NH2:1][C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[C:6]([CH3:13])[C:5]=1[O:14][CH3:15]

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 3475262-Methoxy-1-methyl-3,5-dinitrobenzeneHCID 178418361HCID 178418361, compound

Product 1

HCID 20389417HCID 20389417, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 962WaterSolvent

Procedure

105 g of 2,4-dinitro-6-methylanisole, 1.35 l of ethanol, 150 ml of water and 1 g of Pd/C (5% strength) were initially introduced into the autoclave and hydrogenated at 50° C. with a hydrogen pressure of 50 bar for 12 h. Subsequently, the mixture was cooled and then poured into 1.0 l of semiconcentrated HCl. The catalyst was filtered off, and the filtrate was evaporated to dryness on a rotary evaporator. The residue was extracted by boiling with 2×150 ml of ethanol, filtered off and dried overnight under reduced pressure.

Workup

  1. temperatureSubsequently, the mixture was cooled
  2. filtrationThe catalyst was filtered off
  3. customthe filtrate was evaporated to dryness on a rotary evaporator
  4. extractionThe residue was extracted
  5. filtrationfiltered off
  6. customdried overnight under reduced pressure

Sources & evidence

ORD record
ord-84ea0ca979854fbdb360bb8afb5c4e89
Source dataset
uspto-grants-2007_05
Patent number
US07211119B2

Reaction notes

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