HCID 18003361, compound → HCID 18003354, compound

HRID 478976Notes

Reaction equation

HRID 478976 reaction equation
[CH3:1][C:2]1([CH3:18])[NH:7][C:6]([CH3:9])([CH3:8])[CH2:5][N:4]([CH2:10][CH2:11][O:12][CH2:13][CH2:14][C:15]#[N:16])[C:3]1=[O:17]>CO.[Ni]>[CH3:1][C:2]1([CH3:18])[NH:7][C:6]([CH3:8])([CH3:9])[CH2:5][N:4]([CH2:10][CH2:11][O:12][CH2:13][CH2:14][CH2:15][NH2:16])[C:3]1=[O:17]

Participants

4

Reactant 1

HCID 18003361HCID 18003361, compound

Product 1

HCID 18003354HCID 18003354, compound

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 887MethanolSolvent

Procedure

215.9 g (0.85 moles) of 3-[2-(3,3,5,5-tetramethyl-2-oxo-piperazin-1-yl)-ethoxy]-propionitrile are dissolved in 900 m of methanol and hydrogenated at 120° C. and at 50 bars in the presence of 100 g of Ni Raney as catalyst. The mixture is then filtered and the organic phase is evaporated under vacuum (40° C./1 0 mbar). The residue is distilled giving a white oil b.p. 130-136OC./0.8 mbar.

Workup

  1. filtrationThe mixture is then filtered
  2. customthe organic phase is evaporated under vacuum (40° C./1 0 mbar)
  3. distillationThe residue is distilled
  4. customgiving a white oil b.p

Sources & evidence

ORD record
ord-05a9f82ac0f444b28a2a375a219592b9
Source dataset
uspto-grants-2003_11
Patent number
US06642383B2

Reaction notes

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