Reaktion #93227

Reaktionsgleichung

Chlorocarbonyl isocyanate

N-[4-(6-chlorobenzothiazol-2-yloxyl)phenyl]-N'-methylurea

→

1-[4-(6-chlorobenzothiazol-2-yloxy)phenyl]-3-methyl-1,3,5-triazine-2,4,6-(1H,3H,5H)-trione

Ausbeute 72.5%

Lösungsmittel

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated at the boiling point for 5 hours
2. 2
   SonstigeThe mixture was evaporated under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue was dissolved in a minimal volume of boiling 1,4-dioxane
4. 4
   workup.ADDITIONAfter addition of ethanol (50 ml)
5. 5
   Temperaturthe clear solution was cooled in a refrigerator
6. 6
   FiltrationThe resulting solid substance was collected by filtration
7. 7
   Waschenwashed with cold ethanol
8. 8
   Sonstigedried

Vorschrift

Chlorocarbonyl isocyanate (0.8 g) was added to a suspension of N-[4-(6-chlorobenzothiazol-2-yloxyl)phenyl]-N'-methylurea (2.4 g) in 1,4-dioxane (50 ml), and the mixture was heated at the boiling point for 5 hours. The mixture was evaporated under reduced pressure and the residue was dissolved in a minimal volume of boiling 1,4-dioxane. After addition of ethanol (50 ml), the clear solution was cooled in a refrigerator. The resulting solid substance was collected by filtration, washed with cold ethanol and dried to give 2.1 g of 1-[4-(6-chlorobenzothiazol-2-yloxy)phenyl]-3-methyl-1,3,5-triazine-2,4,6-(1H,3H,5H)-trione of melting point 270°-271°C.

Quelle