HCID 66746000, compound → HCID 66745571, compound

HRID 1810115Notes

Reaction equation

HRID 1810115 reaction equation
[N+:1]([C:4]1[CH:22]=[CH:21][C:7]([O:8][C:9]2[CH:10]=[N:11][N:12]([C:14]3[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=3)[CH:13]=2)=[CH:6][CH:5]=1)([O-])=O>C(O)C.[Fe]>[C:17]1([CH3:20])[CH:16]=[CH:15][C:14]([N:12]2[CH:13]=[C:9]([O:8][C:7]3[CH:21]=[CH:22][C:4]([NH2:1])=[CH:5][CH:6]=3)[CH:10]=[N:11]2)=[CH:19][CH:18]=1

Participants

4

Reactant 1

HCID 66746000HCID 66746000, compound

Product 1

HCID 66745571HCID 66745571, compound

Reagents, catalysts & solvents 2

HCID 23925IronCatalystHCID 702EthanolSolvent

Conditions

Temperature
27.5 °C

Procedure

4-(4-Nitro-phenoxy)-1-p-tolyl-1H-pyrazole (600 mg, 2.03 mml) was taken in ethanol and iron powder (1.13 g, 20.33 mmol) was added and stirred at 20-35° C. for 6 hours. Iron powder was removed and ethanol was evaporated under vacuum. Residue was taken up in water and pH was adjusted to 7 using saturated NaHCO3 solution. The aqueous layer was extracted with ethyl acetate, was washed with brine solution and dried over anhydrous Na2SO4. The solvent was evaporated under vacuum at 50° C. and the product was dried in high vacuum.

Workup

  1. customIron powder was removed
  2. customethanol was evaporated under vacuum
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. washwas washed with brine solution
  5. dry with materialdried over anhydrous Na2SO4
  6. customThe solvent was evaporated under vacuum at 50° C.
  7. customthe product was dried in high vacuum

Sources & evidence

ORD record
ord-20546bdc3f6544a2b4a8a5351f9e0b5c
Source dataset
uspto-grants-2013_01
Patent number
US08362064B2

Reaction notes

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