Process for synthesizing liquid crystal compounds containing 1,3-dioxane
A technology for dioxane and liquid crystal compounds, which is applied in the field of compound synthesis, can solve the problems of high operation risk, high price, fire, etc., and achieves the effects of safe operation, easy storage and simple feeding method.
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[0036] Example 1
[0037] In this example, the compound of formula (I) is diethyl butylmalonate, and butyl propylene glycol is prepared by hydrogenation reduction reaction to illustrate the hydrogenation reduction reaction of alkyl ethyl succinate.
[0038]
[0039] Mix 216 g of potassium borohydride, 170 g of anhydrous lithium chloride and 1500 ml of tetrahydrofuran, cool with ice water for external use, and add dropwise a mixed solution of 216 g of diethyl butylmalonate and 200 ml of tetrahydrofuran. After the addition is complete, the reaction mixture is heated to reflux and reacted for 8-20 hours, monitoring the complete reaction of the raw materials. Pour the reaction solution slowly into 2kg of crushed ice and 1L of deionized water, then add 500ml of petroleum ether and stir for 10 minutes, separate the organic phase and extract the aqueous phase twice with petroleum ether, combine the organic phases, wash with deionized water until neutral, and dry , The solvent was remov...
Example Embodiment
[0045] Example 2
[0046] The obtained alkyl propylene glycol is reacted with the compound of formula (III) to obtain a liquid crystal compound containing 1,3-dioxane.
[0047]
[0048] 117 g of butyl propylene glycol obtained in Example 1, 6 g of p-toluenesulfonic acid, 115 g of p-cyanobenzaldehyde and 800 ml of toluene were mixed. Stir and heat at 110°C to reflux and separate water for 4 hours until no water droplets are formed. Cool down to 50℃, wash with water to neutrality, dry with anhydrous sodium sulfate, remove the solvent under reduced pressure, recrystallize twice with 400ml of absolute ethanol to obtain white crystals of 4-(5-butyl-1,3-dioxane Alkane-2-)benzonitrile (1).
[0049] Yield: 162 g (75% of theory), GC: 99.60%, melting point: 44.4°C, clearing point: 34.8°C.
[0050] According to the similar method described above, the following monomer liquid crystals can be obtained:
[0051] 4-(5-ethyl-1,3-dioxane-2-)benzonitrile;
[0052] 4-(5-propyl-1,3-dioxane-2-)benzo...
Example Embodiment
[0071] Example 3
[0072] In this example, butyl propylene glycol is prepared by hydrogenation reduction of the compound of formula (b) to illustrate the hydrogenation reduction reaction of alkylcyclohexyl ethyl succinate.
[0073]
[0074] 216g potassium borohydride, 170g anhydrous lithium chloride and 1500ml tetrahydrofuran were mixed, cooled with ice water for external use, and a mixed solution of 284g compound of formula (2) and 200ml tetrahydrofuran was added dropwise. After the addition is complete, the reaction mixture is heated to reflux and reacted for 8-20 hours, monitoring the complete reaction of the raw materials. Pour the reaction solution slowly into 2kg of crushed ice and 1L of deionized water, then add 500ml of petroleum ether and stir for 10 minutes, separate the organic phase and extract the aqueous phase twice with petroleum ether, combine the organic phases, wash with deionized water until neutral, and dry , The solvent was removed under reduced pressure to ...
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