Calcium Carbonate → HCID 18706700, compound

HRID 1422222Notes

Reaction equation

HRID 1422222 reaction equation
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH2:16]Br)[CH:3]=1.C(=O)([O-])[O-:19].[Ca+2]>O1CCOCC1.O>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH2:16][OH:19])[CH:3]=1

Participants

5

Reactant 2

HCID 10112Calcium CarbonateHCID 23298010HCID 23298010, compound

Product 1

HCID 18706700HCID 18706700, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Procedure

11.5 g (31.85 mmol) of 7-bromo-5-bromomethyl-2,3-dimethoxy-quinoxaline are suspended at 20° C. in 100 ml of dioxane. 16.4 g (164 mmol) of calcium carbonate in 100 ml of water are then added and the mixture is heated at reflux for 24 hours. The dioxane is concentrated by evaporation and 300 ml of dichloromethane are added. The salt is filtered off, the organic phase is washed with brine and concentrated by evaporation and the residue is chromatographed on silica gel with ethyl acetate and hexane (1:1).

Workup

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 24 hours
  3. concentrationThe dioxane is concentrated by evaporation and 300 ml of dichloromethane
  4. additionare added
  5. filtrationThe salt is filtered off
  6. washthe organic phase is washed with brine
  7. concentrationconcentrated by evaporation
  8. customthe residue is chromatographed on silica gel with ethyl acetate and hexane (1:1)

Sources & evidence

ORD record
ord-e8cd4e97f26b4e49a8ca77d9eddbf969
Source dataset
uspto-grants-2000_06
Patent number
US06080743

Reaction notes

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