Water → HCID 18521587, compound

HRID 413720Notes

Reaction equation

HRID 413720 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]([NH:10][CH2:11][C:12]([O:14]CC2C=CC=CC=2)=[O:13])=[O:9])[CH2:4][CH2:3]1.[H][H].O>[Pd].CO>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([C:8]([NH:10][CH2:11][C:12]([OH:14])=[O:13])=[O:9])[CH2:6][CH2:7]1

Participants

6

Reactant 3

HCID 962WaterHCID 18521579HCID 18521579, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 18521587HCID 18521587, compoundYield 92%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

2.36 g of benzyl N-(4-methylpiperazin-1-ylcarbonyl)glycinate are added, at 20° C., under an argon atmosphere, to 0.15 g of 5% palladium on carbon in suspension in 100 cm3 of methanol. After stirring for 2.5 hours at 22° C., under 1.6 bar of hydrogen, 50 cm3 of water are added and the mixture is filtered on Clarcel. The cake is washed with three times 70 cm3 of water at 60° C. The filtrate is then concentrated to dryness under reduced pressure (2.7 kPa) at 50° C. The residue is dried under reduced pressure (2.7 kPa) at 50° C. to give 1.5 g of N-(4-methylpiperazin-1-ylcarbonyl)glycine.

Workup

  1. additionare added
  2. filtrationthe mixture is filtered on Clarcel
  3. washThe cake is washed with three times 70 cm3 of water at 60° C
  4. concentrationThe filtrate is then concentrated to dryness under reduced pressure (2.7 kPa) at 50° C
  5. customThe residue is dried under reduced pressure (2.7 kPa) at 50° C.

Sources & evidence

ORD record
ord-a94d491d7dff4347841cd97e7b53be9a
Source dataset
uspto-grants-2003_05
Patent number
US06569854B1

Reaction notes

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