4-(alpha-Methylbenzyl)resorcinol synthesis

Yield:85-27-8 88%

Reaction Conditions:

in toluene at 95;Sealed tube;Inert atmosphere;Large scale;Concentration;Temperature;

Steps:

1; 1.1; 1.2; 2; 3; 3.1; 3.2; 4 Example 3
(1) Add 50 L of toluene to the reaction vessel, start stirring, and add 39.6 kg (360 mol) of resorcinol (mw: 110.11).0.45 kg of catalyst solid acid H2SO4-SiO2 (by mass ratio H2SO4: SiO2 = 1:1),After sealing, the vacuum was evacuated and replaced with nitrogen three times. Under a nitrogen atmosphere, the reactor was heated to 95 ° C.After the temperature was stable, 15 kg (144 mol) of styrene (mw: 104.15) was slowly dropped.Control the feeding time 1.5-2 hours, keep the reaction for 3 hours,The reaction was completely detected by liquid phase, and the yield was 89%, and the reaction was stopped.
(2) adding 10 liters of toluene to the reaction solution,Recovery of solid acid H2SO4-SiO2 catalyst by hot filtration,The filtrate was slowly cooled to 0 ° C under stirring, and solid resorcinol was precipitated, filtered, and solid resorcinol was washed with 12 liters (6 liters of X 2 times) of toluene for recovery.The filtrate was concentrated until a solid precipitated, and 10 liters of a mixed solvent (by volume ratio, n-hexane: toluene = 1:1) was heated to 75 ° C to dissolve sufficiently.After cooling to -5 ° C under stirring, crystals were precipitated, and the mixture was kept for 2 hours until the crystals were completely precipitated, followed by pressure filtration, and the obtained solid was washed twice with 20 liters of a mixed solvent (by volume ratio, n-hexane: toluene = 1:1).The resulting solid was dried under vacuum at 50 ° C.It has a white crystal of 24.2 kg and a liquid phase detection content of 98.4%.The product yield is 88%, and the product has a melting point of 76-78 °C.

References:

Liaoning University;Zhou Yunpeng;Zhang Qiushi CN109534960, 2019, A Location in patent:Paragraph 0018; 0025-0041

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