Diethyl Oxalate → HCID 3412732, compound

HRID 1683145Notes

Reaction equation

HRID 1683145 reaction equation
[CH2:1]([N:3]([CH2:8][CH3:9])[CH2:4][CH2:5][CH2:6][NH2:7])[CH3:2].[C:10](OCC)(=[O:16])[C:11]([O:13][CH2:14][CH3:15])=[O:12]>>[CH2:1]([N:3]([CH2:8][CH3:9])[CH2:4][CH2:5][CH2:6][NH:7][C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[O:16])[CH3:2]

Participants

3

Reactant 2

HCID 7268Diethyl OxalateHCID 61011N,N-Diethyl-1,3-propanediamine

Product 1

HCID 3412732HCID 3412732, compound

Procedure

13.0 g of N,N-diethyl-1,3-diaminopropane were added to 70 ml of diethyl oxalate with stirring at room temperature over a period of 20 minutes. After stirring at room temperature for 2 hours, excess diethyl oxalate was distilled off under reduced pressure to obtain 21.7 g of N,N-diethyl-N'-ethoxalyl-1,3-diaminopropane as an oily product. 6.90 g of this oily product and 3.99 g of 3-(2-methoxyethoxy)propylamine were dissolved in 30 ml of methanol and the solution was heated under reflux for 1 hour. The solvent was distilled off under reduced pressure to obtain 9.51 g of Compound B-1 as an oily product.

Workup

  1. stirringAfter stirring at room temperature for 2 hours
  2. distillationexcess diethyl oxalate was distilled off under reduced pressure

Sources & evidence

ORD record
ord-7aeec8524db84b6ba61a9e6b3af0c5ec
Source dataset
uspto-grants-1997_06
Patent number
US05637439

Reaction notes

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