Methylhydrazine → HCID 22105867, compound

HRID 1456004Notes

Reaction equation

HRID 1456004 reaction equation
C(N(CC)CC)C.[CH3:8][NH:9][NH2:10].[CH2:11]([N:13]1[C:18](S(C)=O)=[C:17]([C:22]#[N:23])[C:16](=[O:24])[N:15]2[N:25]=[CH:26][CH:27]=[C:14]12)[CH3:12]>C(O)C>[NH2:23][C:22]1[C:17]2[C:16](=[O:24])[N:15]3[N:25]=[CH:26][CH:27]=[C:14]3[N:13]([CH2:11][CH3:12])[C:18]=2[N:9]([CH3:8])[N:10]=1

Participants

5

Reactant 3

HCID 6061MethylhydrazineHCID 8471TriethylamineHCID 22105859HCID 22105859, compound

Product 1

HCID 22105867HCID 22105867, compoundYield 64%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
60 °C

Procedure

Triethylamine (1.44 g) and methylhydrazine (1.44 g) were added to a solution of 3.2 g of 4-ethyl-5-methanesulfinyl-7-oxo-4,7-dihydropyrazolo[1,5-a]pyrimidine-6-carbonitrile in 100 ml of ethanol and stirred at 60° C. for 30 minutes. The reaction mixture was cooled and the crystals precipitated were collected by filtration and sequentially washed with ethanol, methanol and diethyl ether to provide 1.9 g of the title compound as colorless crystals. The structure and melting point of the compound obtained are shown in Table 1.

Workup

  1. temperatureThe reaction mixture was cooled
  2. customthe crystals precipitated
  3. filtrationwere collected by filtration
  4. washsequentially washed with ethanol, methanol and diethyl ether

Sources & evidence

ORD record
ord-31beed955d084bf2b5388e56c8a7f764
Source dataset
uspto-grants-1998_12
Patent number
US05843951

Reaction notes

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