A kind of synthetic method of cyclohexyl modified cucurbit ring
A synthetic method and a cyclohexyl technology are applied in the field of new synthetic routes of cyclohexyl cucurbit rings, can solve problems such as low reaction yield, cumbersome reaction steps, pollute the environment, and the like, achieve improved yield, overcome cumbersome reaction steps, reduce The effect of pollution
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Embodiment 1
[0026] Step 1: Synthesis of 1,2--Dicyclohexanone Hemihydrate
[0027] Measure the concentrated nitric acid of 104.3ml and add in the three-necked flask, add an appropriate amount of catalyst (V 2 o 5 ) When brown gas is released in the bottle, put it in an ice-salt bath to cool down, control the temperature at -5-20°C, take 52ml of cyclohexanol in the dropper, slowly drop the cyclohexanol into the nitric acid , During the dropping process, the temperature is controlled at 10-15°C, and the drop is completed within 2 hours. After the drop of cyclohexanol is finished and the temperature drops below 0°C, blow air to the liquid surface for 2-4 hours. Washed three times with hot water at 75-80°C to obtain white solid 1,2-cyclohexanedione hemihydrate with a yield of 42%;
[0028] Step 2: Synthesis of cyclohexyl glycoluril
[0029] Take 2.4g of 1,2-cyclohexanedione hemihydrate and 4.8g of urea in a 200mL round neck flask, add 60mL of water and 30mL of ethanol to improve the solubi...
Embodiment 2-20
[0035] A method for cyclohexyl modified cucurbit ring, the difference between embodiment 2-20 and embodiment 1 is that the reaction conditions in step 2 are different acids or different temperatures, as shown in the table:
[0036] Synthesis of Cyclohexyl Glycoluril in Different Acids or Same Acids at Different Temperatures
[0037]
[0038] Using acid to provide protons to make them protonated is beneficial to promote the dehydration of hemihydrate, so that 1,2-cyclohexanedione hemihydrate and urea can be synthesized into glycoluril. Using hydrochloric acid as a proton agent, it can be seen from the above table that using the controlled variable method and using temperature as a variable, the yield of glycoluril shows an increasing trend from 41.40% to 96.60% as the temperature rises from room temperature to 65°C. ℃ showed a steady trend, too high temperature is not conducive to the control of the reaction, so it is most appropriate to choose the reaction at 65 ℃. Using s...
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