Sulfuric Acid → HCID 853977, compound

HRID 2243773Notes

Reaction equation

HRID 2243773 reaction equation
[CH3:1][NH:2][C:3]([NH2:5])=[O:4].[C:6]([CH2:9][C:10](=O)[CH3:11])(=O)[CH3:7].S(=O)(=O)(O)O>C(O)C>[CH3:1][N:2]1[C:6]([CH3:7])=[CH:9][C:10]([CH3:11])=[N:5][C:3]1=[O:4]

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 11719MethylureaHCID 31261Acetylacetone

Product 1

HCID 853977HCID 853977, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

20.0 g (0.262 mol) of N-methylurea and 29.4 g (0.291 mol) of acetylacetone were together dissolved in 100 ml of absolute ethanol. 97 g of concentrated sulfuric acid were then added, and the reaction mixture heated up. The mixture was then after-stirred for 1 hour at room temperature. After just a short time, the hydrogen sulfate salt of the product precipitated out in the form of a pale, crystalline solid, which was filtered off. This salt was dissolved in a small amount of water and the solution was rendered neutral using 10% strength sodium hydroxide solution. Extraction was then carried out by shaking with chloroform, and the solvent was dried with magnesium sulfate. After removing the solvent on a rotary evaporator, the desired product was produced in the form of pale pink-colored crystals.

Workup

  1. temperaturethe reaction mixture heated up
  2. customAfter just a short time, the hydrogen sulfate salt of the product precipitated out in the form of a pale, crystalline solid, which
  3. filtrationwas filtered off
  4. dissolutionThis salt was dissolved in a small amount of water
  5. extractionExtraction
  6. stirringby shaking with chloroform
  7. dry with materialthe solvent was dried with magnesium sulfate
  8. customAfter removing the solvent
  9. customon a rotary evaporator

Sources & evidence

ORD record
ord-4f3de9942df5416aa8c8ba1ca29fcd41
Source dataset
uspto-grants-2010_03
Patent number
US07678156B2

Reaction notes

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