반응 #449868

반응 방정식

resorcinol

aluminium trichloride

2-mesityl-4,6-dichloro-1,3,5-triazine

2-Mesityl-4,6-dichloro-1,3,5-triazine

HCl

→

title product ( ii )

수율 84.6%

2-Mesityl-4,6-bis(2,4-dihydroxyphenyl)-1,3,5-triazine

수율 84.6%

용매

sulfolane

—

petroleum ether

sulfolane

반응 조건

후처리

1. 1
   workup.ADDITIONDuring this addition
2. 2
   기타warms to 45° C
3. 3
   기타The upper phase (petroleum ether) is removed
4. 4
   workup.ADDITIONstill hot into a stirred mixture of 2.11 of methanol and 2.11 of water
5. 5
   여과the solid is filtered off
6. 6
   workup.STIRRINGstirred in 2.2 l of 1 molar HCl for 1 hour
7. 7
   여과re-filtered
8. 8
   workup.STIRRINGstirred for 30 minutes
9. 9
   여과re-filtered
10. 10
    기타The filter cake is dried for 24 hours at 80° C.

실험 절차

148.7 g (1.21 mol) of anhydrous aluminium trichloride (purity 98%) are added with stirring to a suspension of 130.0 g (0.485 mol) of 2-mesityl-4,6-dichloro-1,3,5-triazine (i) in 300 ml of petroleum ether with a boiling range of 110°-140° C. and 385 ml of sulfolane. During this addition, the mixture warms to 45° C. A solution of 133.5 e (1.21 mol) of resorcinol (purity 98%) in 155 ml of sulfolane is added to the mixture over the course of 45 minutes. The mixture is warmed at 80°-85° C. for 5 hours 30 minutes with evolution of HCl. The upper phase (petroleum ether) is removed, and the lower, viscous phase is transferred while still hot into a stirred mixture of 2.11 of methanol and 2.11 of water. After the mixture has been stirred for 14 hours, the solid is filtered off, stirred in 2.2 l of 1 molar HCl for 1 hour and re-filtered. The filter cake is suspended in 1000 ml of water, stirred for 30 minutes and re-filtered. This operation is repeated twice. The filter cake is dried for 24 hours at 80° C. and a pressure of 60 mmHg (8000 Pa), giving 170.5 g of the title product (ii) of the formula ##STR62## of m.p. 230°-234° C.

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