Sulfuric Acid → HCID 19734103, compound

HRID 326965Notes

Reaction equation

HRID 326965 reaction equation
[C:1]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O[S:16](O)(=O)=O>>[O:8]=[C:1]1[CH:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[S:16][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]1=2

Participants

3

Reactant 2

HCID 1118Sulfuric AcidHCID 7170Ethyl benzoylacetate

Product 1

HCID 19734103HCID 19734103, compoundYield 114.3%

Conditions

Temperature
5 °C

Procedure

Ethyl benzoylacetate (100.0 g, 0.52 mol) was added dropwise over a period of 1.5 h under vigorous mechanical stirring to fuming H2SO4 37% (500.0 g) cooled at 5° C. in an ice bath. After the addition was complete the reaction mixture was stirred for 1.5 h and then added to 1000 g of ice. The solid product was collected by filtration and washed with cold water (30 ml) to give 132.1 g (85%) of Compound X as a pale yellow solid:melting point 138°-140° C.

Workup

  1. additionAfter the addition
  2. filtrationThe solid product was collected by filtration
  3. washwashed with cold water (30 ml)

Sources & evidence

ORD record
ord-f3c05adc92b3415d9542ba14d2f1e077
Source dataset
uspto-grants-1993_12
Patent number
US05272032

Reaction notes

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