1-Methylpiperazine → HCID 13048624, compound

HRID 364008Notes

Reaction equation

HRID 364008 reaction equation
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=[C:2]1[CH:10](Cl)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH3:18][N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>O1CCOCC1>[CH3:18][N:19]1[CH2:24][CH2:23][N:22]([CH:10]([C:2]2[O:1][C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[CH:3]=2)[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:21][CH2:20]1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 13048623HCID 13048623, compound

Product 1

HCID 13048624HCID 13048624, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Conditions

Temperature
70 °C

Procedure

25.4 g of α(benzofuran-2-yl)benzyl chloride dissolved in 150 ml of dioxane are added slowly at about 60°-70° C. to 26 g of 1-methyl-piperazine in 150 ml of dioxane. After the addition, the mixture is stirred at about 70° C. for a further two hours. The solvent is removed under reduced pressure, the residue is then dissolved in 5% sodium bicarbonate and extracted with ethyl ether. After washing the ether phase with water and drying with sodium sulphate, the hydrochloride is precipitated by bubbling in anhydrous hydrochloric acid gas: M.P. 186°-188° C. (isopropanol).

Workup

  1. additionAfter the addition
  2. customThe solvent is removed under reduced pressure
  3. dissolutionthe residue is then dissolved in 5% sodium bicarbonate
  4. extractionextracted with ethyl ether
  5. washAfter washing the ether phase with water
  6. dry with materialdrying with sodium sulphate
  7. customthe hydrochloride is precipitated
  8. customby bubbling in anhydrous hydrochloric acid gas

Sources & evidence

ORD record
ord-51b89a2863bb445fb8380f8c65971d5e
Source dataset
uspto-grants-1986_08
Patent number
US04604392

Reaction notes

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