Water → o-Carbamoyl-alpha-(1-piperazinyl)acetanilide dihydrochloride

HRID 1381189Notes

Reaction equation

HRID 1381189 reaction equation
[ClH:1].Cl.[C:3]([C:6]1[CH:28]=[CH:27][CH:26]=[CH:25][C:7]=1[NH:8][C:9](=[O:24])[CH2:10][N:11]1[CH2:16][CH2:15][N:14](CC2C=CC=CC=2)[CH2:13][CH2:12]1)(=[O:5])[NH2:4].O>[C].[Pd].CO>[ClH:1].[ClH:1].[C:3]([C:6]1[CH:28]=[CH:27][CH:26]=[CH:25][C:7]=1[NH:8][C:9](=[O:24])[CH2:10][N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1)(=[O:5])[NH2:4]

Participants

5

Reactant 2

HCID 962WaterHCID 23323546o-Carbamoyl-alpha-(4-benzyl-1-piperazinyl)acetanilide dihydrochloride

Product 1

HCID 23323544o-Carbamoyl-alpha-(1-piperazinyl)acetanilide dihydrochloride

Reagents, catalysts & solvents 2

HCID 178418390HCID 178418390, compoundCatalystHCID 887MethanolSolvent

Procedure

50 Grams of o-carbamoyl-α-(4-benzyl-1-piperazinyl)acetanilide dihydrochloride, 4 g of 10%-palladium carbon, 70 ml of water and 300 ml of methanol were mixed together and the mixture was subjected to catalytic reduction at a room temperature. Then the catalyst was removed from the mother liquor, and the mother liquor was concentrated to dryness. The residue obtained was crystallized by adding acetone, and recrystallized from water-acetone to obtain 35.2 g of o-carbamoyl-α-(1-piperazinyl)acetanilide dihydrochloride. Colorless cotton fiber-like crystals. Melting point: 239.5°-242° C. (decomposed).

Workup

  1. customwas subjected to catalytic reduction at a room temperature
  2. customThen the catalyst was removed from the mother liquor
  3. concentrationthe mother liquor was concentrated to dryness
  4. customThe residue obtained
  5. customwas crystallized
  6. additionby adding acetone
  7. customrecrystallized from water-acetone

Sources & evidence

ORD record
ord-061e8e3a43bd40c9a67e4ffdd8c6e4d1
Source dataset
uspto-grants-1986_04
Patent number
US04585774

Reaction notes

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