Sulfuric Acid → HCID 22899237, compound

HRID 1018755Notes

Reaction equation

HRID 1018755 reaction equation
OS(O)(=O)=O.[CH3:6][C:7]([CH3:25])=[CH:8][CH2:9][C:10]1[C:20](=[O:21])[C:19]2[CH:18]=[CH:17][C:16]([O:22][CH3:23])=[CH:15][C:14]=2[C:12](=[O:13])[C:11]=1[OH:24]>>[CH3:6][C:7]1([CH3:25])[O:21][C:20]2[C:19]3[CH:18]=[CH:17][C:16]([O:22][CH3:23])=[CH:15][C:14]=3[C:12]([C:11](=[O:24])[C:10]=2[CH2:9][CH2:8]1)=[O:13]

Participants

3

Reactant 2

HCID 1118Sulfuric AcidHCID 178487262HCID 178487262, compound

Product 1

HCID 22899237HCID 22899237, compoundYield 96.2%

Procedure

Concentrated H2SO4 (25 mL) was added to compound 52 (2.454 g) at 20° C. After stirring for 20 min, the mixture was diluted with ice water (500 mL). The resulting red precipitate 54 was collected by filtration, washed with water, and dried in vacuo. It was obtained as a red powder (2.36 g, 96%): 1H NMR (CDCl3) δ7.72 (1H, d, J=8.6 Hz), 7.56 (1H, d, J=2.7 Hz), 7.12 (1H, dd, J=8.6, 2.7 Hz), 3.90 (3H,S), 2.55 (2H, t, J=6.7 Hz), 1.84 (2H, t, J=6.7 Hz), 1.46 (6H, S).

Workup

  1. filtrationThe resulting red precipitate 54 was collected by filtration
  2. washwashed with water
  3. customdried in vacuo

Sources & evidence

ORD record
ord-2b74f747f1614e2ba783779f510bf4d3
Source dataset
uspto-grants-2002_11
Patent number
US06482943B1

Reaction notes

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