Method for synthesizing 4-[2-(trans-4-alkyl cyclohexyl )ethyl]cyclohexanone
A synthesis method and alkyl ring technology are applied in the synthesis of liquid crystal materials, in the field of synthesis of 4-[2-(trans-4-alkylcyclohexyl)ethyl]cyclohexanone, which can solve the problem of lithium aluminum hydride reagents. High price, environmental pollution and other problems, to achieve the effect of reducing raw material consumption, avoiding serious environmental pollution, and high total yield
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Example Embodiment
[0062] Example 1: Preparation of 4-[2-(trans-4-pentylcyclohexyl)ethyl]cyclohexanone
[0063] The specific preparation steps of this embodiment are as follows:
[0064] Step 1: Synthesis of trans-4-pentylcyclohexylcarbaldehyde (B)
[0065] Under nitrogen protection, add 52.2g (0.6mol) morpholine and 300mL toluene into a 1000mL three-necked flask, cool to -5℃ with ice salt water while stirring, and add 150g (0.52mol) red aluminum toluene solution dropwise, in which the mass fraction of red aluminum 70%), after the addition, keep the reaction at -5~0℃ for 2 hours to prepare reducing reagent.
[0066] Under the protection of nitrogen, 42.5g (0.2mol) trans-4-pentylcyclohexyl methyl ester and 50mL toluene were added to a 1000mL three-necked flask, and the temperature was cooled to -5°C with an ice salt bath while stirring, and the above-prepared product was added dropwise After the addition of the reducing reagent, keep the reaction temperature between -5°C and 0°C for 2 hours. After the ...
Example Embodiment
[0076] Example 2: Preparation of 4-[2-(trans-4-ethylcyclohexyl)ethyl]cyclohexanone
[0077] The preparation method is the same as that in Example 1, except that trans-4-ethylcyclohexyl methyl ester is used instead of trans-4-pentylcyclohexyl methyl ester to prepare the target product 4-[2-(trans- 4-Ethylcyclohexyl)ethyl]cyclohexanone. The melting point is 40.2°C.
Example Embodiment
[0078] Example 3: Preparation of 4-[2-(trans-4-propylcyclohexyl)ethyl]cyclohexanone
[0079] The preparation method is the same as that in Example 1, except that trans-4-propylcyclohexyl methyl ester was used instead of trans-4-pentylcyclohexyl methyl ester to prepare the target product 4-[2-(trans- 4-propylcyclohexyl)ethyl]cyclohexanone. The melting point is 45.5°C.
[0080] Other Examples: Preparation of 4-[2-(trans-4-propylcyclohexyl)ethyl]cyclohexanone
[0081] The preparation method is the same as that of Example 1, except that the organic solvent N,N-dimethylformamide described in step (4) is replaced with dichloromethane, dichloroethane, toluene, acetone, and ethanol. The target product 4-[2-(trans-4-propylcyclohexyl)ethyl]cyclohexanone can be prepared.
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