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Hydrogen Peroxide → HCID 178513609, Verbindung

HRID 1524864
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1524864
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]=[C:11]([CH:14]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:15]([O:17]C)=[O:16])[NH:12][CH:13]=2)=[CH:5][CH:4]=1)#[N:2].C(=O)([O-])[O-:27].[K+].[K+].OO.[O-2].[Mg+2]>CS(C)=O>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([C:9]2[N:10]=[C:11]([CH:14]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:15]([OH:17])=[O:16])[NH:12][CH:13]=2)=[CH:7][CH:8]=1)(=[O:27])[NH2:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 784Hydrogen PeroxideHCID 11430Potassium CarbonateHCID 6850729Magnesium monoxideHCID 178499804HCID 178499804, Verbindung

Produkt 1

HCID 178513609HCID 178513609, VerbindungAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679
Dimethyl Sulfoxide
Lösungsmittel

Reaktionsbedingungen

Temperatur
2.5 °C

Versuchsvorschrift

The product from Example 56 Part A (0.99 g, 3.0 mmol) was dissolved in 10 mL of DMSO. Potassium carbonate (1.24 g, 9.0 mmol) was added. The mixture was cooled to 0-5° C. and 30% H2O2 (3.18 mL of 30% aqueous solution) was added, followed by magnesium oxide (0.24 g, 15 mmol). The cooling bath was removed and the mixture was stirred at RT under N2 for 4 h. The mixture was filtered to remove inorganic material. Water (30 mL) was added to the filtrate and the resulting mixture was stirred at rt for 40 min. The mixture was acidified with 1N HCl to pH 5. The precipitate formed was filtered and dried to afford 0.67 g of the acid (67%). MS 336.30 (M+H)+.

Aufarbeitung

  1. customThe cooling bath was removed
  2. filtrationThe mixture was filtered
  3. customto remove inorganic material
  4. additionWater (30 mL) was added to the filtrate
  5. stirringthe resulting mixture was stirred at rt for 40 min
  6. customThe precipitate formed
  7. filtrationwas filtered
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e8046466f7c9498b85c243d04e4247e2
Quelldatensatz
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09079860B2

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