Ethanol → HCID 10888189, compound

HRID 2377229Notes

Reaction equation

HRID 2377229 reaction equation
C=O.[C:3](=[O:6])([O-])[O-].[K+].[K+].[CH3:9][N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.[CH2:16](O)[CH3:17]>>[CH2:16]([O:6][CH2:3][N:13]1[CH2:14][CH2:15][N:10]([CH3:9])[CH2:11][CH2:12]1)[CH3:17]

Participants

5

Reactant 4

HCID 702EthanolHCID 712FormaldehydeHCID 11430Potassium CarbonateHCID 531671-Methylpiperazine

Product 1

HCID 10888189HCID 10888189, compound

Procedure

To a suspension of paraformaldehyde and potassium carbonate in ethanol at about 0° C. was added 1-methylpiperazine dropwise. The mixture was stirred vigorously at room temperature for about 67 hours and filtered. The filter cake was washed with diethyl ether and the combined filtrates were concentrated under vacuum. The residue was distilled under reduced pressure (30° C. at 2.5 Torr) to provide the desired product. 1H NMR (500 MHz, DMSO-d6): δ 1.09 (t, J=6.8 Hz, 3H), 2.14 (s, 3H), 2.28 (m, 4H), 2.56 (m, 4H), 3.40 (q, J=6.8 Hz, 2H), 3.96 (s, 2H).

Workup

  1. filtrationfiltered
  2. washThe filter cake was washed with diethyl ether
  3. concentrationthe combined filtrates were concentrated under vacuum
  4. distillationThe residue was distilled under reduced pressure (30° C. at 2.5 Torr)

Sources & evidence

ORD record
ord-ca126561ed81486da38a0fc427529011
Source dataset
uspto-grants-2008_12
Patent number
US07468371B2

Reaction notes

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