Methylhydrazine → HCID 21484120, compound

HRID 1414878Notes

Reaction equation

HRID 1414878 reaction equation
[Cl:1][C:2]1[C:3](=[O:20])[N:4]([C:9]2[CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[CH:11][C:10]=2[F:19])[N:5]=[CH:6][C:7]=1Cl.[CH3:21][NH:22][NH2:23]>CO>[Cl:1][C:2]1[C:3](=[O:20])[N:4]([C:9]2[CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[CH:11][C:10]=2[F:19])[N:5]=[CH:6][C:7]=1[N:22]([CH3:21])[NH2:23]

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 214841184,5-Dichloro-2-[2-fluoro-5-(trifluoromethyl)phenyl]pyridazin-3(2H)-one

Product 1

HCID 21484120HCID 21484120, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 41.8 grams of 4,5-dichloro-2-(2-fluoro-5-trifluoromethylphenyl)-pyridazin-3(2H)-one in 400 grams of methanol cooled to 15° C is added dropwise 18.4 grams of methylhydrazine. The reaction mixture is stirred at room temperature for 4 hours, and evaporated to dryness below 30° C. The resulting precipitate is dissolved in 300 grams of methylene dichloride and washed with 300 grams of water. The organic phase is separated and evaporated to dryness. The solid is crystallized from methanol to yield the title compound, m.p. 128° to 130° C (decomposition).

Workup

  1. customevaporated to dryness below 30° C
  2. dissolutionThe resulting precipitate is dissolved in 300 grams of methylene dichloride
  3. washwashed with 300 grams of water
  4. customThe organic phase is separated
  5. customevaporated to dryness
  6. customThe solid is crystallized from methanol

Sources & evidence

ORD record
ord-fa34b16539a54e73a0269036989edf01
Source dataset
uspto-grants-1977_01
Patent number
US04002751

Reaction notes

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