1-Methylpiperazine → HCID 13769984, compound

HRID 542711Notes

Reaction equation

HRID 542711 reaction equation
[CH3:1][C:2]1[S:11][C:10]2[C:9](=[O:12])[NH:8][C:7]3[CH:13]=[CH:14][CH:15]=[N:16][C:6]=3[N:5]([C:17](=[O:20])[CH2:18]Cl)[C:4]=2[CH:3]=1.[CH3:21][N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1>O1CCOCC1CCO>[CH3:1][C:2]1[S:11][C:10]2[C:9](=[O:12])[NH:8][C:7]3[CH:13]=[CH:14][CH:15]=[N:16][C:6]=3[N:5]([C:17](=[O:20])[CH2:18][N:25]3[CH2:26][CH2:27][N:22]([CH3:21])[CH2:23][CH2:24]3)[C:4]=2[CH:3]=1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 13769983HCID 13769983, compound

Product 1

HCID 13769984HCID 13769984, compound

Reagents, catalysts & solvents 1

HCID 23496530HCID 23496530, compoundSolvent

Procedure

A suspension of the product obtained in (a) (5 g) and N-methylpiperazine (4.3 ml) in dioxane-ethanol 9:1 (50 ml) is heated to reflux for 2 hours. After cooling and filtration of the insoluble impurities, the clear filtrate is evaporated and the residue dissolved in chloroform (100 ml). The solution is washed with a diluted ammonium hydroxyde solution (20 ml), dried, decolorized and evaporated. The residue, crystallized from methanol, yields 2.2 g of the title product, melting at 273°-275° C. (dec.).

Workup

  1. additionA suspension of the product
  2. temperatureis heated
  3. temperatureto reflux for 2 hours
  4. temperatureAfter cooling
  5. filtrationfiltration of the insoluble impurities
  6. customthe clear filtrate is evaporated
  7. dissolutionthe residue dissolved in chloroform (100 ml)
  8. washThe solution is washed with a diluted ammonium hydroxyde solution (20 ml)
  9. customdried
  10. customevaporated
  11. customThe residue, crystallized from methanol

Sources & evidence

ORD record
ord-53f97d812239416ab46c9d8008370bf5
Source dataset
uspto-grants-1987_04
Patent number
US04659707

Reaction notes

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