Methylhydrazine → HCID 74220801, compound

HRID 588636Notes

Reaction equation

HRID 588636 reaction equation
Cl[C:2]1[N:3]=[N:4][C:5]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[C:6]([Cl:16])[C:7]=1[C:8]([C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)=O.[CH3:23][NH:24][NH2:25]>C(O)C>[Cl:16][C:6]1[C:5]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[N:4][N:3]=[C:2]2[N:24]([CH3:23])[N:25]=[C:8]([C:10]3[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=3)[C:7]=12

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 86717328HCID 86717328, compound

Product 1

HCID 74220801HCID 74220801, compoundYield 31.1%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
60 °C

Procedure

A mixture of (3,5-dichloro-6-phenyl-pyridazin-4-yl)-(3-pyridyl)methanone (100 mg, 0.3 mmol) and methyl hydrazine (19.5 mg, 0.42 mmol) in ethanol (1.5 mL) was stirred in a sealed tube at 60° C. for 3 h. The reaction mixture was concentrated in vacuo and the residue was purified by column chromatography (silica gel, isohexane/ethyl acetate 9:1 to 8:2) yielding Compound 26 as a solid (30 mg).

Workup

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue was purified by column chromatography (silica gel, isohexane/ethyl acetate 9:1 to 8:2)

Sources & evidence

ORD record
ord-165a35fca59d4f6482cbf982e862cf55
Source dataset
uspto-grants-2016_01
Patent number
US09227976B2

Reaction notes

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