Sulfuric Acid → HCID 178468373, compound

HRID 2306143Notes

Reaction equation

HRID 2306143 reaction equation
S(=O)(=O)(O)O.[C:6]([CH2:9][C:10](=[O:12])[CH3:11])(=[O:8])[CH3:7].[N:13]([O-])=[O:14].[Na+]>>[CH3:11][C:10](=[O:12])[C:9](=[N:13][OH:14])[C:6](=[O:8])[CH3:7]

Participants

4

Reactant 3

HCID 1118Sulfuric AcidHCID 31261AcetylacetoneHCID 23668193Sodium Nitrite

Product 1

HCID 178468373HCID 178468373, compoundYield 96%

Conditions

Temperature
17.5 °C

Procedure

Variant a): In a stirred vessel, 21 l of 20% strength sulfuric acid and 6 kg (60 mol) of acetylacetone were initially charged. The mixture was cooled to about 17° C. and, at 15-20° C., 4.2 kg (60.84 mol) of 40.5% strength aqueous sodium nitrite solution were metered in. The mixture was subsequently stirred at about 17° C. for another 20 minutes and then extracted with 25 l of ethyl acetate. The organic phase was concentrated under reduced pressure, giving 7.42 kg (96% yield) of the title compound.

Workup

  1. extractionextracted with 25 l of ethyl acetate
  2. concentrationThe organic phase was concentrated under reduced pressure

Sources & evidence

ORD record
ord-93fb51ce83c846e2a2bdbc192965c9c3
Source dataset
uspto-grants-2002_08
Patent number
US06441236B1

Reaction notes

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