반응 #4609

반응 방정식

methanol

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

2-nitrobenzoylisocyanate

water

→

desired product

수율 84.5%

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

수율 84.5%

용매

dioxane

dioxane

반응 조건

후처리

1. 1
   기타Into a flask, a solution obtained
2. 2
   workup.ADDITIONwas introduced
3. 3
   기타a solution obtained
4. 4
   workup.ADDITIONwas dropwise added
5. 5
   기타the mixture was reacted at room temperature for 9 hours
6. 6
   기타After the completion of the reaction
7. 7
   여과subjected to filtration
8. 8
   세척washed with hot water
9. 9
   기타The crystals thereby obtained
10. 10
    여과subjected to filtration again

실험 절차

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.

출처