Carbon Dioxide → HCID 54019971, compound

HRID 1729721Notes

Reaction equation

HRID 1729721 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[C:8]([CH2:10][C:11](O)=O)#[N:9].C=O.[C:16](=O)=O>O.O1CCOCC1>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:16][C:10](=[CH2:11])[C:8]#[N:9])[CH2:4][CH2:3]1

Participants

7

Reactant 4

HCID 280Carbon DioxideHCID 712FormaldehydeHCID 9740Cyanoacetic acidHCID 531671-Methylpiperazine

Product 1

HCID 54019971HCID 54019971, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Procedure

0.5 Mole of N-methylpiperazine are added to 0.5 mole of cyanoacetic acid in 150 cc. of dioxan at a temperature kept at around 0° C. This is followed by the addition of 1 mole of formaldehyde in the form of a 30% aqueous solution. After the heat effect has abated, the mixture is stirred until there is no further evolution of carbon dioxide gas (approximately 2 hours). 200 cc. of water are then added, the product extracted with ether, dried over sodium sulphate and the ether removed in vacuo, followed by distillation.

Workup

  1. customkept at around 0° C
  2. extractionthe product extracted with ether
  3. dry with materialdried over sodium sulphate
  4. customthe ether removed in vacuo
  5. distillationfollowed by distillation

Sources & evidence

ORD record
ord-c1704f1f3ddc4d2eacefb814dcd41d45
Source dataset
uspto-grants-1976_11
Patent number
US03989722

Reaction notes

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