HCID 6414556, compound → HCID 21388244, compound

HRID 1834024Notes

Reaction equation

HRID 1834024 reaction equation
[CH3:1][O:2][C:3]1[N:4]=[N+:5]([O-])[C:6]2[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:7]=2[N:8]=1.[H][H]>[Ni].C(O)C>[CH3:1][O:2][C:3]1[N:4]=[N:5][C:6]2[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:7]=2[N:8]=1

Participants

5

Reactant 2

HCID 6414556HCID 6414556, compoundHCID 178418361HCID 178418361, compound2×

Product 1

HCID 21388244HCID 21388244, compound

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 702EthanolSolvent

Procedure

21.2 g (0.1 mole) of 3-methoxy-7-chloro-benzo-1,2,4-triazine 1-oxide and 5 g of Raney nickel in 150 ml of ethanol were initially introduced into a stirred VA autoclave. A pressure of 15 atmospheres of hydrogen was applied at 30° C. The mixture was stirred at 30° to 50° C for 5 hours and during this time further hydrogen was fed in under pressure until the pressure remained constant. The autoclave was let down, the catalyst was filtered off and the filtrate was evaporated in vacuo. The residue was recrystallized from wash benzine. 15.2 g. that is to say 78% of theory, of 3-methoxy-7-chlorobenzo-1,2,4-triazine with a melting point of 122° C were obtained.

Workup

  1. customwas applied at 30° C
  2. filtrationthe catalyst was filtered off
  3. customthe filtrate was evaporated in vacuo
  4. customThe residue was recrystallized
  5. washfrom wash benzine

Sources & evidence

ORD record
ord-e8a8d1efd39c4089a1c01f785eb05397
Source dataset
uspto-grants-1978_01
Patent number
US04067981

Reaction notes

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