Hydrochloric Acid → N,N-Diethyl-4-phenylpiperazine-1-carboxamide--hydrogen chloride (1/1)

HRID 543475Notes

Reaction equation

HRID 543475 reaction equation
[C:1]1([N:7]2[CH2:12][CH2:11][N:10]([C:13](=[O:19])[N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:20]>C(Cl)(Cl)Cl>[ClH:20].[C:1]1([N:7]2[CH2:8][CH2:9][N:10]([C:13](=[O:19])[N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH2:11][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 423348HCID 423348, compound

Product 1

HCID 20461509N,N-Diethyl-4-phenylpiperazine-1-carboxamide--hydrogen chloride (1/1)Yield 70.9%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

In 50 ml of chloroform was dissolved 2.6 g (0.01 mole) of 1-phenyl-4-diethylcarbamoylpiperazine at room temperature, and the solution was saturated with gaseous hydrogen chloride and stirred for a certain time. The solvent was removed by distillation under reduced pressure. Then, 50 ml of acetone was added to the residue and the mixture was stirred for a certain time. The precipitated crystal was recovered by filtration, washed with acetone, stirred in 50 ml of acetone to effect washing and dried to obtain 2.1 g of 1-phenyl-4-diethylcarbamoylpiperazine hydrochloride having a melting point of 190° to 192° C. The yield was 70.9%. The elementary analysis values are as follows.

Workup

  1. customThe solvent was removed by distillation under reduced pressure
  2. additionThen, 50 ml of acetone was added to the residue
  3. stirringthe mixture was stirred for a certain time
  4. filtrationThe precipitated crystal was recovered by filtration
  5. washwashed with acetone
  6. stirringstirred in 50 ml of acetone
  7. washto effect washing
  8. customdried

Sources & evidence

ORD record
ord-9d2b228f5648472cbe6fa64313a46713
Source dataset
uspto-grants-1984_05
Patent number
US04446133

Reaction notes

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