2-Methylpiperazine → HCID 19350778, compound

HRID 1636279Notes

Reaction equation

HRID 1636279 reaction equation
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([C:13]([F:16])([F:15])[F:14])[C:11]=1F)[N:8]([CH3:17])[CH:7]=[C:6]([C:18]([OH:20])=[O:19])[C:5]2=[O:21].[CH3:22][CH:23]1[CH2:28][NH:27][CH2:26][CH2:25][NH:24]1>N1C=CC=CC=1>[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([C:13]([F:15])([F:16])[F:14])[C:11]=1[N:27]1[CH2:26][CH2:25][NH:24][CH:23]([CH3:22])[CH2:28]1)[N:8]([CH3:17])[CH:7]=[C:6]([C:18]([OH:20])=[O:19])[C:5]2=[O:21]

Participants

4

Reactant 2

HCID 660572-MethylpiperazineHCID 19350779HCID 19350779, compound

Product 1

HCID 19350778HCID 19350778, compoundYield 78.5%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Conditions

Temperature
105 °C

Procedure

In 30 ml of pyridine were dissolved 1.5 g (0.0049 mole) of 6,7-difluoro-8-trifluoromethyl-1,4-dihydro-1-methyl-4-oxoquinoline-3-carboxylic acid and 1.5 g (0.015 mole) of 2-methylpiperazine, the mixture was stirred at 105° C. for 3 hours, and then the solvent was removed by evaporation under reduced pressure. Ethanol was added to the residue, precipitated crystals were collected by filtration, the crystals obtained were washed with ethanol and dried, and then 1.49 g of 6-fluoro-8-trifluoromethyl-1,4-dihydro-4-oxo-1-methyl-7-(3-methylpiperazin-1-yl)quinoline-3-carboxylic acid was obtained as yellow powder.

Workup

  1. customthe solvent was removed by evaporation under reduced pressure
  2. additionEthanol was added to the residue
  3. customprecipitated crystals
  4. filtrationwere collected by filtration
  5. customthe crystals obtained
  6. washwere washed with ethanol
  7. customdried

Sources & evidence

ORD record
ord-b573874a441c4d1a9b6920da37f1d567
Source dataset
uspto-grants-2000_03
Patent number
US06034086

Reaction notes

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