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Sulfamic Acid → 6,7-Bis(ethoxycarbonyloxy)chromone-3-carboxylic acid

HRID 67091
Notes
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Reaction equation

HRID 67091 reaction equation
[CH2:1]([O:3][C:4]([O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[O:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[O:13][CH:12]=[C:11]([CH:23]=[O:24])[C:10]2=[O:25])=[O:5])[CH3:2].S(=O)(=O)([OH:28])N.Cl([O-])=O.[Na+]>ClCCl.O>[CH2:1]([O:3][C:4]([O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[O:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[O:13][CH:12]=[C:11]([C:23]([OH:28])=[O:24])[C:10]2=[O:25])=[O:5])[CH3:2]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 3

HCID 5987Sulfamic AcidHCID 128006236,7-Bis(ethoxycarbonyloxy)chromone-3-carboxaldehydeHCID 23668197Sodium Chlorite

Product 1

HCID 128006246,7-Bis(ethoxycarbonyloxy)chromone-3-carboxylic acid

Reagents, catalysts & solvents 2

HCID 962WaterSolvent2×
HCID 6344
Dichloromethane
Solvent

Procedure

The compound (1.05 g) obtained in (2) was dissolved in of dichloromethane (31.5 ml) and a solution of 1.05 g of sulfamic acid in water (18.9 ml) was added at 10° C. with stirring. Then, a solution of sodium chlorite (525.6 mg) in water (1.2 ml) was added. The solution was stirred at the same temperature for 1 hour, and allowed to separate. The dichloromethane layer was washed with water (once) and then with a saturated aqueous solution of sodium chloride (twice), and dried over magnesium sulfate. The solvent was distilled off, and ethyl ether was added to the residue to triturate it. The triturated product was collected by filtration, and dried to afford the desired product (950 mg).

Workup

  1. stirringThe solution was stirred at the same temperature for 1 hour
  2. customto separate
  3. washThe dichloromethane layer was washed with water (once) and then with a saturated aqueous solution of sodium chloride (twice), and
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was distilled off
  6. additionethyl ether was added to the residue
  7. customto triturate it
  8. filtrationThe triturated product was collected by filtration
  9. customdried

Sources & evidence

ORD record
ord-4af7f5458ec34fecb17cc608fbfb5e95
Source dataset
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04344944

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes