Methylhydrazine → HCID 12562816, compound

HRID 1413930Notes

Reaction equation

HRID 1413930 reaction equation
Cl[C:2]1[N:3]=[N:4][C:5]([N:8]2[C:12]([NH2:13])=[C:11]([C:14](=O)[NH2:15])[CH:10]=[N:9]2)=[CH:6][CH:7]=1.[CH3:17][NH:18][NH2:19]>CN(C)C=O>[CH3:17][N:18]([C:2]1[N:3]=[N:4][C:5]([N:8]2[C:12]([NH2:13])=[C:11]([C:14]#[N:15])[CH:10]=[N:9]2)=[CH:6][CH:7]=1)[NH2:19]

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 12562796HCID 12562796, compound

Product 1

HCID 12562816HCID 12562816, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

A mixture of 2.2 g. (10 mmoles) of 3-chloro-6-(4-cyano-5-amino-1-pyrazolyl)-pyridazine (prepared according to Example 24), 1.38 g. (30 mmoles) of methylhydrazine and 25 ml. of dimethylformamide is heated at 120°-130° C. for 7.5 hours, and after cooling the mixture is poured onto ice. The separated crystals are filtered, washed with water and triturated with 5 ml. of hot ethanol, filtered and dried. Yield: 2.1 g. (91%); m.p.: 260° C. (with decomposition).

Workup

  1. additionA mixture of 2.2 g
  2. temperatureafter cooling the mixture
  3. additionis poured onto ice
  4. filtrationThe separated crystals are filtered
  5. washwashed with water
  6. customtriturated with 5 ml
  7. filtrationof hot ethanol, filtered
  8. customdried

Sources & evidence

ORD record
ord-a7bd6a4de44a4c4c8515c9b56dc0580f
Source dataset
uspto-grants-1981_02
Patent number
US04251658

Reaction notes

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