Hydrogen Peroxide → 5,6-bis(4-methoxyphenyl)-1,2,4-triazin-3(2h)-one

HRID 889830Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 889830
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)=[N:13][NH:12][C:11](=S)[N:10]=2)=[CH:5][CH:4]=1.[OH-:24].[Na+].OO>O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)=[N:13][NH:12][C:11](=[O:24])[N:10]=2)=[CH:5][CH:4]=1

Komponenten

5

Edukt 3

HCID 784Hydrogen Peroxide2×HCID 14798Sodium HydroxideHCID 42600365,6-bis-(4-methoxyphenyl)-1,2,4-triazin-3-thione

Produkt 1

HCID 2310985,6-bis(4-methoxyphenyl)-1,2,4-triazin-3(2h)-oneAusbeute 94,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A slurry of 9.6 g of 5,6-bis-(4-methoxyphenyl)-1,2,4-triazin-3-thione (29.5 mmol) in 100 mL of water was treated with 2.64 g of 50% aqueous sodium hydroxide (33 mmol). Most of the solids dissolved. The reaction mixture was cooled in an ice bath and 3.8 g of 30% hydrogen peroxide (33 mmol) was added slowly. An additional 4 mL of hydrogen peroxide solution was added, and the reaction mixture was stirred overnight at room temperature. The solids were filtered, washed with water, and dried under vacuum to give 8.6 g of product, mp 238–242° C.

Aufarbeitung

  1. dissolutionMost of the solids dissolved
  2. temperatureThe reaction mixture was cooled in an ice bath
  3. filtrationThe solids were filtered
  4. washwashed with water
  5. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f46f46b796a44dfa844749a081aa6281
Quelldatensatz
uspto-grants-2006_02
Patentnummer
US06995157B2

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