Ethylamine → HCID 19898758, compound

HRID 1196718Notes

Reaction equation

HRID 1196718 reaction equation
[CH2:1]([NH2:3])[CH3:2].[N:4]1([C:7]2[N:12]([CH3:13])[C:11](=[O:14])[N:10]([CH3:15])[C:9](=[O:16])[CH:8]=2)[CH2:6][CH2:5]1>>[CH3:13][N:12]1[C:7]([NH:4][CH2:6][CH2:5][NH:3][CH2:1][CH3:2])=[CH:8][C:9](=[O:16])[N:10]([CH3:15])[C:11]1=[O:14]

Participants

3

Reactant 2

HCID 6341EthylamineHCID 10397412HCID 10397412, compound

Product 1

HCID 19898758HCID 19898758, compound

Procedure

To 7.6 g of a 70% aqueous ethylamine solution was added 0.91 g of the previously obtained Compound 12, followed by stirring at room temperature for 3 hours. After completion of the stirring treatment, the reaction solution was concentrated under reduced pressure, and 80 ml of ethanol were added to the resultant residue. Then, the ethanol solution was further concentrated under reduced pressure. Ether was added to the resultant residue, and crystallization was then effected. Afterward, a mixed solution of ether and hexane in a ratio of 1:1 (volume ratio) was added thereto. The crystals were then collected by filtration to obtain 1.07 g of N-(1,3-dimethyl-2,4-dioxopyrimidine-6-yl)-N'-ethylethylene-diamine (Compound 13).

Workup

  1. concentrationAfter completion of the stirring treatment, the reaction solution was concentrated under reduced pressure, and 80 ml of ethanol
  2. additionwere added to the resultant residue
  3. concentrationThen, the ethanol solution was further concentrated under reduced pressure
  4. additionEther was added to the resultant residue, and crystallization
  5. additionAfterward, a mixed solution of ether and hexane in a ratio of 1:1 (volume ratio) was added
  6. filtrationThe crystals were then collected by filtration

Sources & evidence

ORD record
ord-ddd5349b7e3c4d0a8ff851c74f0d9bf3
Source dataset
uspto-grants-1992_05
Patent number
US05114941

Reaction notes

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