Synthesis method for dibenzoxazole compounds
A synthesis method and benzoxazole technology are applied in the synthesis field of bisbenzoxazole compounds, can solve the problems of long reaction time, unfavorable environment, large amount of alkali, etc., and achieve short reaction time, less three wastes and low cost Effect
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example 1
[0035] 11.5 g (0.05 mol) of 4,4'-dicyanostyrene, 16 g (0.11 mol) of o-aminophenol hydrochloride, and 90 g of nitrobenzene were respectively put into a 150 ml three-necked bottle. Sealed, vacuumed, replaced with nitrogen. Raise the temperature to 190-200°C, stir rapidly and keep warm for 3 hours, and the reaction is completed. Cool down, filter and dry. 19.5 g of 4,4'-bis(benzoxazol-2-yl)stilbene was obtained.
example 2
[0037] 9 g (0.05 mol) of naphthalene-1,4-dinitrile, 16 g (0.11 mol) of o-aminophenol hydrochloride, and 90 g of sulfolane were respectively put into a 150 ml three-necked flask. Sealed, vacuumed, replaced with nitrogen. Raise the temperature to 200-230° C., stir rapidly and keep warm for 3 hours, and the reaction is completed. 17 g of 1,4-bis(benzoxazol-2-yl)naphthalene was obtained.
example 3
[0039] In a 150ml three-necked bottle, 11.5g (0.05mol) of 4,4'-dicyano-stilbene, 8g (0.055mol) of o-aminophenol hydrochloride, and 8.8g (0.055mol) of o-amino-p-cresol hydrochloride ), sulfolane 80g. Sealed, vacuumed, replaced with nitrogen. Raise the temperature to 190-200°C, stir rapidly and keep warm for 3 hours, and the reaction is completed. Cool down, filter and dry. 19 g of a bisbenzoxazole stilbene mixture was obtained.
[0040] Determine the percentage composition of the mixture with liquid chromatography as:
[0041] 4-(Benzoxazol-2-yl)-4'-(5-methylbenzoxazol-2-yl)stilbene 49%; 4,4'-bis(benzoxazol-2- base) stilbene 24%; 4,4'-bis(5-methylbenzoxazol-2-yl) stilbene 27%.
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