Reaktion #4609

Reaktionsgleichung

methanol

4-(5-bromo-2-pyrimidinyloxy)-3-chloroaniline

2-nitrobenzoylisocyanate

water

→

desired product

Ausbeute 84.5%

N-(2-nitrobenzoyl)-N'-[4-(5-bromo-2-pyrimidinyloxy)-3-chlorophenyl]urea

Ausbeute 84.5%

Lösungsmittel

dioxane

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeInto a flask, a solution obtained
2. 2
   workup.ADDITIONwas introduced
3. 3
   Sonstigea solution obtained
4. 4
   workup.ADDITIONwas dropwise added
5. 5
   Sonstigethe mixture was reacted at room temperature for 9 hours
6. 6
   SonstigeAfter the completion of the reaction
7. 7
   Filtrationsubjected to filtration
8. 8
   Waschenwashed with hot water
9. 9
   SonstigeThe crystals thereby obtained
10. 10
    Filtrationsubjected to filtration again

Vorschrift

Into a flask, a solution obtained by dissolving 6.80 g of the above 4-(5-bromo-2-pyrimidinyloxy)-3-chloroaniline in 30 ml of dioxane, was introduced, and a solution obtained by dissolving 5.76 g of 2-nitrobenzoylisocyanate in 30 ml of dioxane, was dropwise added thereto, and then the mixture was reacted at room temperature for 9 hours. After the completion of the reaction, the product was poured into water, subjected to filtration and washed with hot water. The crystals thereby obtained were put into methanol, and stirred, and then subjected to filtration again, to obtain 9.42 g of the desired product having a melting point of from 234 to 236° C.

Quelle