Sodium Chloride → HCID 11481213, compound

HRID 456584Notes

Reaction equation

HRID 456584 reaction equation
[Cl-].[Na+].[OH:3][CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([S:12][CH2:13][C:14](O)=[O:15])=[C:8]([N+:17]([O-])=O)[CH:7]=1>C(O)C.[Fe]>[OH:3][CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]2[S:12][CH2:13][C:14](=[O:15])[NH:17][C:8]=2[CH:7]=1

Participants

5

Reactant 2

HCID 5234Sodium ChlorideHCID 11459551HCID 11459551, compound

Product 1

HCID 11481213HCID 11481213, compoundYield 46.5%

Reagents, catalysts & solvents 2

HCID 23925IronCatalystHCID 702EthanolSolvent2×

Procedure

A mixture of iron powder (1.24 g, 22 mmol) and sodium chloride (1.24 g, 21 mmol) in 50% aqueous ethanol (25 ml) was heated under reflux for 15 minutes. A solution of crude (g) (0.92 g, 3.6 mmol) in ethanol (5 ml) was then added quickly and the reaction mixture was heated under reflux for 2 hours. The mixture was filtered through keiselguhr and the solution was evaporated to dryness. The residue was dissolved in water and acidified to pH5 with 1M aqueous hydrochloric acid. The precipitate was collected by filtration, washed with water, then dried to give a white solid (0.35 g, 46%).

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 15 minutes
  3. temperaturethe reaction mixture was heated
  4. temperatureunder reflux for 2 hours
  5. filtrationThe mixture was filtered through keiselguhr
  6. customthe solution was evaporated to dryness
  7. dissolutionThe residue was dissolved in water
  8. filtrationThe precipitate was collected by filtration
  9. washwashed with water
  10. customdried

Sources & evidence

ORD record
ord-73eef3fb97ed4264be4833ce8d04a325
Source dataset
uspto-grants-2007_03
Patent number
US07186730B2

Reaction notes

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