Synthesis method of thiodiethylene bis [3-(3, 5-di-tert-butyl-4-hydroxyphenyl) propionate]
A technology of di-tert-butylphenol and di-tert-butyl, which is applied in the field of synthesis of thiodiethylenebis[3-propionate], can solve the problems of cumbersome synthesis process operation, production constraints, and low yield. Achieve the effects of simple process, high purity and high product purity
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Embodiment 1
[0046] Under a nitrogen atmosphere, add 50 mmol (10.3 g) of 2,6-di-tert-butylphenol into the reactor, heat up to 80°C to melt, then add 5 mmol (0.56 g) of potassium tert-butoxide in 15 ml of o-di Solution in toluene; reflux for 30min, the solution gradually turns light green. The temperature of the solution was raised to 125°C, and 50 mmol (4.3 g, 4.5 ml) of methyl acrylate was slowly added dropwise, and the reaction was stirred for 2.5 h, and the solution turned into light yellow. Then the temperature was lowered to 100°C, 50mmol (4.0g, 3.4ml) of 2-chloroethanol was slowly added dropwise, stirred and reacted for 4h, then stopped. The reaction product was cooled to room temperature, washed 3 times with water, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized from ethyl acetate to obtain the intermediate 3-(3,5-di-tert-butyl - 14.9 g of 2-chloroethyl 4-tetrahydroxyphenyl)propanoate (yield 87.6%). ESI-MS:...
Embodiment 2
[0049] Under nitrogen atmosphere, add 50mmol (10.3g) of 2,6-di-tert-butylphenol into the reactor, heat up to 80°C to melt, then add 6mmol (0.67g) of potassium tert-butoxide in 15ml of o-di Solution in toluene; reflux for 30min, the solution gradually turns light green. The solution was warmed up to 130°C, 55mmol (4.7g, 5ml) of methyl acrylate was slowly added dropwise, and the reaction was stirred for 2h, and the solution turned into light yellow. Then the temperature was lowered to 105°C, 55mmol (4.4g, 3.7ml) of 2-chloroethanol was slowly added dropwise, stirred and reacted for 3.5h, then stopped. The reaction product was cooled to room temperature, washed 3 times with water, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized from ethyl acetate to obtain the intermediate 3-(3,5-di-tert-butyl - 15.3 g of 2-chloroethyl 4-tetrahydroxyphenyl)propanoate (90.2% yield).
[0050] 20mmol (6.8g) of intermediate 3...
Embodiment 3
[0052] Under a nitrogen atmosphere, add 100mmol (20.6g) of 2,6-di-tert-butylphenol into the reactor, heat up to 80°C to melt it, then add 30mmol (3.36g) of potassium tert-butoxide in 40ml of o-di Solution in toluene; reflux for 30min, the solution gradually turns light green. The solution was warmed up to 120°C, 100 mmol (8.6 g, 9.0 ml) of methyl acrylate was slowly added dropwise, and the reaction was stirred for 2 h, and the solution turned into light yellow. Then the temperature was lowered to 95°C, 100mmol (8.0g, 6.8ml) of 2-chloroethanol was slowly added dropwise, stirred and reacted for 4.5h, then stopped. The reaction product was cooled to room temperature, washed 3 times with water, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized from ethyl acetate to obtain the intermediate 3-(3,5-di-tert-butyl - 29.5 g of 2-chloroethyl 4-tetrahydroxyphenyl)propionate (yield 86.9%).
[0053] 60mmol (20.4g) of...
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