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

HRID 223130
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 223130
[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]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×
HCID 6344
Dichloromethane
Lösungsmittel

Versuchsvorschrift

The compound (1.05 g) obtained in (b) of Experimental Example 1 was dissolved in 31.5 ml of dichloromethane, and a solution of 1.05 g of sulfamic acid in 18.9 ml of water was added at 10° C. with stirring. Then, a solution of 525.6 mg of sodium chlorite in 1.2 ml of water 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 solidify it. The solidified product was collected by filtration, and dried to afford 950 mg of the desired product.

Aufarbeitung

  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. filtrationThe solidified product was collected by filtration
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-0b980d29728140d99b3cab0db5d4f2c8
Quelldatensatz
uspto-grants-1982_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04352801

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