Methylhydrazine → HCID 70493454, compound

HRID 465103Notes

Reaction equation

HRID 465103 reaction equation
[IH:1].CS[C:4]1[NH:5][CH2:6][CH2:7][N:8]=1.[CH3:9][NH:10][NH2:11]>C(O)C>[IH:1].[CH3:9][NH:10][NH:11][C:4]1[NH:5][CH2:6][CH2:7][N:8]=1

Participants

4

Procedure

A 12.2 g portion of 2-methylthioimidazoline, hydroiodide was dissolved in 30 ml of ethanol. A 5.32 ml portion of methyl hydrazine was added dropwise over 1/2 hour. This mixture was refluxed overnight, then chilled in an ice bath. The solvent was evaporated and the residue triturated with ether and refrigerated overnight. The mxture was evaporated to an oil which was dissolved in methanol and added to 400 ml of ether. The resulting solid was collected, dissolved in hot methanol and poured into 100 ml of ether. The resulting solid was collected, giving 4,5-dihydro-2-(2-methylhydrazino)-1H-imidazole, hydroiodide.

Workup

  1. temperatureThis mixture was refluxed overnight
  2. temperaturechilled in an ice bath
  3. customThe solvent was evaporated
  4. customthe residue triturated with ether and refrigerated overnight
  5. customThe mxture was evaporated to an oil which
  6. dissolutionwas dissolved in methanol
  7. additionadded to 400 ml of ether
  8. customThe resulting solid was collected
  9. dissolutiondissolved in hot methanol
  10. additionpoured into 100 ml of ether
  11. customThe resulting solid was collected

Sources & evidence

ORD record
ord-941e4cfe68f54a99a7b40d44f15af35b
Source dataset
uspto-grants-1985_10
Patent number
US04550169

Reaction notes

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