Benzaldehyde → Benzaldehyde Methylhydrazone

HRID 1908688Notes

Reaction equation

HRID 1908688 reaction equation
[CH3:1][NH:2][NH2:3].[CH:4](=O)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>C(OCC)C>[CH3:1][NH:2][N:3]=[CH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Participants

4

Reactant 2

HCID 240BenzaldehydeHCID 6061Methylhydrazine

Product 1

HCID 302615Benzaldehyde Methylhydrazone

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

18.4 g (0.4 mol) of methylhydrazine were initially charged in 248.7 g of diethyl ether. At 22-26° C., 42.4 g (0.4 mol) of benzaldehyde were added dropwise within 1.75 hours. The reaction mixture was then stirred at reflux temperature for 5 hours. The residue obtained after the solvent had been distilled off was taken up in diethyl ether and the solution was dried over sodium sulfate. After drying, the solution was concentrated under reduced pressure and the residue obtained was distilled at 78° C./0.5-1 mbar.

Workup

  1. temperatureat reflux temperature for 5 hours
  2. customThe residue obtained after the solvent
  3. distillationhad been distilled off
  4. dry with materialthe solution was dried over sodium sulfate
  5. customAfter drying
  6. concentrationthe solution was concentrated under reduced pressure
  7. customthe residue obtained
  8. distillationwas distilled at 78° C./0.5-1 mbar

Sources & evidence

ORD record
ord-4539ebc5479445bc84cab04ec7eeaeee
Source dataset
uspto-grants-2013_12
Patent number
US08598222B2

Reaction notes

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