3,5-Dihydroxybenzyl alcohol synthesis

6synthesis methods

Product Name:3,5-Dihydroxybenzyl alcohol
CAS Number:29654-55-5
Molecular formula:C7H8O3
Molecular Weight:140.14

Preparation of 3,5-dihydroxybenzyl alcohol: Add 50mL THF to a 250mL three-necked flask, add 3.15g (0.082mol) NaBH, 2.38g (0.01mol) 3,5-Diacetoxybenzoic acid, control the temperature at 0 degrees in an ice-water bath, slowly drop 60ml THF solution containing 9g (0.036mol) I2, and then add 4.76g (0.02mol) of the product from the previous step after the dropwise addition, heat to reflux, and track the reaction with a plate. After the reaction is completed, concentrate to dryness under reduced pressure, add 100mL saturated NaHCO solution, extract with ether, combine the organic layers, dry with anhydrous magnesium sulfate, filter, concentrate, and recrystallize with hot water to obtain 3.5g white crystals with a yield of 83.2%.

99-10-5 Synthesis

99-10-5
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29654-55-5
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Yield:29654-55-5 85%

Reaction Conditions:

with sodium tetrahydroborate;Trimethyl borate;dimethyl sulfate in tetrahydrofuran at 20; for 5.5 h;

Steps:

1.1 A method for synthesizing 3,5-dihydroxybenzaldehyde, comprising the following steps

step 1,Under the protection of nitrogen,Dimethyl sulfate (2 kg) was added dropwise to a solution of sodium borohydride (615 g) in tetrahydrofuran (1 kg) at 0 ° C for 1 hour.Stirring at 0 ° C for 1 hour, then stirring at room temperature for 4 hours until the mixture was free of gas;Further, a solution of 3,5-dihydroxybenzoic acid (1 kg) and trimethyl borate (2 kg) in tetrahydrofuran (1 kg) was added dropwise thereto, and the mixture was added dropwise for 0.5 hour, and stirred at room temperature for 5 hours;After the reaction is over, keep the system at 0 °C.Deionized water (1 kg) was added thereto and stirred for 0.5 hours.Tetrahydrofuran was distilled off at 50 ° C using a rotary evaporator, followed by extraction with ethyl acetate (2 kg).Then, wash back three times with saturated sodium bicarbonate solution (2 kg each time), and wash the backwash 3 times with saturated brine (2 kg each time).Finally, it was dried and concentrated at 45 ° C using a rotary evaporator.Obtained white solid B (770 g), yield 85%

References:

CN110256214,2019,A Location in patent:Paragraph 0030-0037