Methanesulfonic Acid → 1-(2',6'-Dimethylphenyl)-4-methylamino-1,2-dihydro-1,3,5-triazin-2-one methanesulfonate

HRID 1395428Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1395428
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]1[CH:14]=[N:13][CH:12]([NH:15][CH3:16])[NH:11][C:10]1=[O:17].[CH3:18][S:19]([OH:22])(=[O:21])=[O:20]>O>[CH3:18][S:19]([OH:22])(=[O:21])=[O:20].[CH3:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[C:3]=1[N:9]1[CH:14]=[N:13][C:12]([NH:15][CH3:16])=[N:11][C:10]1=[O:17]

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 705842081-(2,6-Dimethylphenyl)-4-methylamino-dihydro-1,3,5-triazin-2-one

Produkt 1

HCID 204573291-(2',6'-Dimethylphenyl)-4-methylamino-1,2-dihydro-1,3,5-triazin-2-one methanesulfonateAusbeute 94,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 6.0 g (0.026 moles) of 1-(2,6-dimethylphenyl)-4-methylamino-dihydro-1,3,5-triazin-2-one in 100 ml iPA was prepared with warming. To the warm solution was added 2.0 ml (0.031 moles) of methane-sulfonic acid. The mixture became hot and crystals of white crystalline solid began to form almost immediately. The mixture allowed to cool to room temperature in tap water and filtered. The solution was washed with iPA/Et2O to give 8.00 g of product which was dried overnight at 50°-60° C. in a vacuum. Obtained 8.0 g of 1-(2,6-dimethylphenyl)-4-methylaminodihydro-1,3,5-triazin-2-one methanesulfonate after drying.

Aufarbeitung

  1. temperaturewith warming
  2. customto form almost immediately
  3. filtrationfiltered
  4. washThe solution was washed with iPA/Et2O

Quellen und Nachweise

ORD-Eintrag
ord-904dff2c04924f57806d41ba2c7c3ffb
Quelldatensatz
uspto-grants-1980_05
Patentnummer
US04203984

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