Reaktion #55857

Reaktionsgleichung

m-ethynylphenol

NaOH

cyanuric chloride

→

bis-(m-ethynylphenoxy)-chloro-1,3,5-triazine

Ausbeute 95.8%

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter stirring for one hour at this temperature
2. 2
   Filtrationthe resulting mixture is filtered
3. 3
   Sonstigeto remove a white solid which
4. 4
   Waschenis washed with water
5. 5
   Sonstigedried in vacuum overnight at 35° C
6. 6
   Temperaturincreases to 127°-128° C. upon one recrystallization from chloroform/heptane

Vorschrift

The bis-(m-ethynylphenoxy)-chloro-1,3,5-triazine is prepared by first adding m-ethynylphenol (11.4 g, 0.097 mole) in 20 ml of a 5 N NaOH dropwise to a stirred solution of cyanuric chloride (9.22 g, 0.05 mole) in 50 ml of acetone with stirring at 15°-18° C. After stirring for one hour at this temperature, the resulting mixture is filtered to remove a white solid which is washed with water and dried in vacuum overnight at 35° C. The yield of the product is 16.14 g (yield of 95.8%). The product has a melting point of 121°-125° C. which increases to 127°-128° C. upon one recrystallization from chloroform/heptane. This product is analyzed by NMR and determined to be bis-(m-ethynylphenoxy)-chloro-1,3,5-triazine represented by the formula:

Quelle