Preparation method of vitamin A ester intermediate C15 and vitamin A ester
A technology for vitamins and intermediates, which is applied in the field of preparation of vitamin A ester intermediate C15 and vitamin A ester, can solve the problems of complicated post-processing, low purity of vitamin A palmitate, unenvironmental protection and the like
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Embodiment 1
[0122] Example 1: 2,6,6-trimethyl-2-chloromethylcyclohexene (Ⅲ 1 ) preparation
[0123] Add 500 g of 1,2-dichloroethane, 154.0 g (1.0 mol) of 3,7-di Methyl-3-hydroxy-1,6-octadiene, 131.0 g (1.1 moles) of thionyl chloride, kept between 40°C and 45°C, stirred for 3 hours, cooled to 10-15°C to obtain chlorinated The reaction liquid was transferred to a constant pressure dropping funnel and set aside. In another 1000 ml four-necked flask equipped with stirring, thermometer, reflux condenser and constant pressure dropping funnel, add 100 g of 1,2-dichloroethane, 5.0 g of 98% concentrated sulfuric acid, and keep it at 70°C to 75°C. Between ℃, add the obtained chlorination reaction liquid dropwise, and the dropwise addition is completed in 2 hours. After that, stir and react at 70℃~75℃ for 3 hours, cool to 10-15℃, add 100 grams of water, stand to separate layers, and distill the organic phase After recovering the solvent, 171.0 grams of colorless liquid 2,6,6-trimethyl-2-chloromet...
Embodiment 2
[0124] Example 2: 2,6,6-trimethyl-2-chloromethylcyclohexene (Ⅲ 1 ) preparation
[0125] Under nitrogen protection, add 500 g of dichloromethane, 154.0 g (1.0 mole) of 3,7-dimethyl Base-3-hydroxyl-1,6-octadiene, 135.6 g (1.3 moles) of 35% hydrochloric acid aqueous solution, kept between 30°C and 35°C, stirred and reacted for 2 hours, cooled to 10-15°C, and separated into layers to obtain The organic phase is the chlorination reaction liquid, which is transferred to a constant-pressure dropping funnel for later use. In another 1000 ml four-necked flask equipped with stirring, thermometer, reflux condenser and constant pressure dropping funnel, add 100 g of dichloromethane, 5.0 g of 98% concentrated sulfuric acid, keep between 35°C and 40°C, drop Add the obtained chlorinated reaction liquid, drop it in 2 hours, after that, stir and react at 35°C to 40°C for 4 hours, cool to 10-15°C, add 100 grams of water, stand to separate layers, and distill the organic phase to recover the s...
Embodiment 3
[0126] Example 3: 2,6,6-trimethyl-2-bromomethylcyclohexene (Ⅲ 2 ) preparation
[0127] Under nitrogen protection, add 500 g of dichloromethane, 154.0 g (1.0 mole) of 3,7-dimethyl Base-3-hydroxy-1,6-octadiene, 220.0 g (1.1 mol) 40% hydrobromic acid aqueous solution, kept between 30°C and 35°C, stirred for 2 hours, cooled to 10-15°C, separated , the organic phase was obtained as a bromination reaction liquid, which was transferred to a constant pressure dropping funnel for subsequent use. In another 1000 ml four-necked flask equipped with stirring, thermometer, reflux condenser and constant pressure dropping funnel, add 100 g of dichloromethane, 5.0 g of 98% concentrated sulfuric acid, keep between 35°C and 40°C, drop Add the obtained bromination reaction liquid, and drop it in 2 hours. After that, stir and react at 35°C to 40°C for 3 hours, cool to 10-15°C, add 100 grams of water, let stand to separate layers, and distill the organic phase to recover the solvent to obtain 19...
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