Method for preparing antiform - 4 - acetoxy - 2 - methyl - butenoic aldehyde
A technology of acetoxy and crotonaldehyde, which is applied in the preparation of pentacyclic unsaturated carbon frame compounds and the field of preparation of trans-4-acetoxy-2-methyl-2-butenal, which can solve the problem of receiving The efficiency cannot reach the yield, the process cost is increased, and the production cost is increased, so as to achieve the effects of reducing reaction steps, easy recycling, and less environmental pollution
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[0014] example 1
[0015] (1) Add 1 mol of isoprene to 2 mol of acetic anhydride solution, stir, cool to -10°C to 0°C, maintain this temperature, and then add 1 mol of tert-butyl hypochlorite dropwise within 1.5 hours. After dripping, the temperature was raised to 80°C, 0.05mol p-toluenesulfonic acid was added to react for 10 hours, 500ml ice water was added after the reaction, the organic phase was separated, dried with 20g anhydrous sodium sulfate and filtered to remove the desiccant. Under 5mmHg, 0.8 mol of chloroester was obtained by distillation, with a content of 93%.
[0016] (2) Add 1mol of chloroester to 500ml of toluene, then add 1mol of hexamethylenetetramine, maintain the temperature at about 40℃, react for 8 hours, then add 500ml of water, heat up to 80℃, and then add 2mol of glacial acetic acid Add dropwise within 2 hours and continue the reaction for 10 hours. After the reaction is completed, the organic phase is separated, dried with 20g anhydrous sodium sulfate, a...
Example
[0017] Example 2
[0018] (1) Add 1 mol of isoprene to 2 mol of acetic anhydride solution, stir, cool to -10 to 0°C, maintain this temperature, and then add 1 mol of tert-butyl hypochlorite dropwise within 1.5 hours. After dripping, the temperature was raised to 80°C, 0.1 mol sulfuric acid was added to react for 10 hours, 500 ml of ice water was added after the reaction, the organic phase was separated, dried with 20 g of anhydrous calcium chloride, and the desiccant was filtered off. At 5mmHg, 0.81 mol of chloroester was obtained by distillation, with a content of 93%.
[0019] (2) Add 1mol of chloroester to 500ml of acetonitrile, then add 1mol of hexamethylenetetramine, keep the temperature at about 40℃, react for 8 hours, then filter, add 500ml of water to the filter cake to dissolve, then add 500ml of 1,2- Dichloroethane was heated to 80°C, then 2mol of glacial acetic acid was added dropwise within 2 hours, and the reaction was continued for 6 hours. After the reaction was com...
Example
[0020] Example 3
[0021] (1) Add 1 mol of isoprene to 2 mol of acetic anhydride solution, stir, cool to -10-0°C, maintain this temperature, and then add 1 mol of tert-butyl hypochlorite dropwise within 1.5 hours. After the dripping is completed, the temperature is raised to 80° C., 0.1 mol nitric acid is added to react for 10 hours, 500 ml of ice water is added after the reaction, the organic phase is separated, dried with 20 g of anhydrous sodium sulfate, and the desiccant is filtered off. Under 5mmHg, 0.78mol of chloroester was obtained by distillation, with a content of 91%.
[0022] (2) Add 1mol of chloroester to 500ml of petroleum ether, then add 1mol of hexamethylenetetramine, maintain the temperature at about 40℃, react for 8 hours, then add 500ml of water, heat up to 90℃, and then add 2mol of ice Acetic acid was added dropwise within 2 hours, and the reaction was continued for 6 hours. After the reaction was completed, the organic phase was separated, dried with 20 g of a...
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