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ChemicalBook CAS DataBase List Bemotrizinol

Bemotrizinol synthesis

5synthesis methods
In a three-necked flask equipped with a stirrer, a thermometer and a condenser, 40.30 g (0.1 mol) of 2,4-bis(2,4-dihydroxyphenyl)-6-(4-methoxyphenyl)-1,3,5-triazine, 29.02 g (0.21 mol) of potassium carbonate and 105 mL of N, N-dimethylformamide were added in sequence, and the temperature was raised to 100°C. Reflux and stir for 30 minutes; add 46.35g (0.24mol) of DMF solution containing isooctane bromide at a uniform rate within 1 hour, continue to reflux and stir at 100°C after the addition is complete, and monitor the reaction progress with a thin layer chromatography; after the reaction of the raw materials is completed, stop stirring, cool to room temperature, filter, add ethyl acetate to the filtrate for extraction, wash with saturated brine, dry the organic phase with anhydrous sodium sulfate, filter, and spin-dry the filtrate to obtain a colourless transparent oil, i.e. 50.4g of a crude product of bis-ethylhexyloxyphenol methoxyphenyl triazine (Bemotrizinol), with a yield of 80.2% and a purity of 89.90% detected by HPLC.
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Yield:-

Steps:

Multi-step reaction with 3 steps
1: aluminum (III) chloride / sulfolane / 40 - 60 °C
2: aluminum (III) chloride / sulfolane / 5 h / 40 - 50 °C
3: sodium carbonate / N,N-dimethyl-formamide / 125 °C

References:

A S Tech Co., Ltd.;Yoon Jong-bae;Park Ho-jun;Nam Ho-tae KR2019/136506, 2019, A

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