Ethylene Glycol → 1-(1,3-Dioxolan-2-yl)-4-methylpiperazine

HRID 223404Notes

Reaction equation

HRID 223404 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH:8]([O:12][CH2:13][CH3:14])[O:9]CC)[CH2:4][CH2:3]1.C(O)CO>C(O)C>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([CH:8]2[O:9][CH2:14][CH2:13][O:12]2)[CH2:6][CH2:7]1

Participants

4

Reactant 2

HCID 174Ethylene GlycolHCID 22167370HCID 22167370, compound

Product 1

HCID 450995721-(1,3-Dioxolan-2-yl)-4-methylpiperazine

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

The amide acetal produced in Example 1 (3.03 g, 0.015 mole) was combined while stirring with ethylene glycol (0.93 g, 0.015 mole) in a glass flask at ambient temperature under nitrogen. The reaction was continued with stirring for 18 hours. The by-product ethanol formed during the reaction was removed by vacuum and the reaction continued for an additional 18 hours with stirring under vacuum. The resulting product was found to have a boiling point of about 220° C., and identified as the desired product by NMR spectroscopy.

Workup

  1. customwas removed by vacuum
  2. waitthe reaction continued for an additional 18 hours
  3. stirringwith stirring under vacuum

Sources & evidence

ORD record
ord-d515cd2706004bef827eb1cc5786e16d
Source dataset
uspto-grants-1982_10
Patent number
US04354028

Reaction notes

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