A kind of method of synthesizing trans-cyclohexanedimethylamine
A technology for aqueous solution of cyclohexyldimethylamine and methylamine, which is applied in the direction of condensation/addition reaction to prepare amino compounds, asymmetric synthesis, organic chemical methods, etc., can solve the problems of messy reaction and unfavorable environment, and achieve low cost and high efficiency. The effect of reaction yield and improvement of core competitiveness
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0017]
[0018] In a reaction bottle with a balloon buffer seal, mix epoxycyclohexane (98.2 g, 1.0 mol) and 25% aqueous methylamine solution (1.02 mol), then add 2.5 g of inorganic boric acid catalyst, and heat up to 50°C for reaction 2 hours, after the reaction is over. Cool down to 0°C, add 50% sulfuric acid solution (1.02 mol) dropwise to the above reaction solution, and control the temperature not to exceed 40°C during the entire dropping process. Heat up to 110°C with stirring to remove water by distillation under normal pressure. When no more water flows out, the reaction system gradually becomes sticky. After adding 85 ml of sulfolane, change to vacuum distillation. At this time, gradually increase the reaction temperature to the final 150°C , Vacuum for 7-8 hours, and detect that the water content is 0.2%. Cool the reaction solution to 0°C, add potassium hydroxide solution dropwise to adjust the pH=12-13, start to gradually heat up with stirring slowly, when the te...
Embodiment 2
[0021]
[0022] In a reaction bottle with a balloon buffer seal, mix epoxycyclohexane (98.2 g, 1.0 mol) and 30% methylamine aqueous solution (1.1 mol), then add 1.4 g of inorganic boric acid catalyst, and heat up to 60 ° C for 1.5 hours, after the reaction is over. Cool down to 0°C, add 50% sulfuric acid solution (1.1 mol) dropwise to the above reaction solution, and keep the temperature within 40°C during the whole dropping process. Heat up to 110°C with stirring to remove water by distillation under normal pressure. When no more water flows out, the reaction system gradually becomes sticky. After adding 95 ml of sulfolane, change to vacuum distillation. At this time, gradually increase the reaction temperature to the final 150°C , Vacuum for 7-8 hours, and detect the water content of 0.26%. Cool the reaction liquid to 0°C, add potassium hydroxide aqueous solution dropwise to adjust the pH=13-14, start to gradually raise the temperature under stirring slowly, when the tem...
Embodiment 3
[0025]
[0026] In a reaction flask with a balloon buffer seal, epoxycyclohexane (98.2 g, 1.0 mol) and 35% methylamine aqueous solution (1.0 mol) were mixed, then 2.5 g of inorganic boric acid catalyst was added, and the temperature was raised to 50°C for reaction 2 hours, after the reaction is over. Cool down to 0°C, add 40% sulfuric acid solution (1.0 mol) dropwise to the above reaction solution, and control the temperature not to exceed 40°C during the entire dropping process. Heat up to 110°C with stirring to remove water by distillation under normal pressure. When the water no longer flows out, the reaction system gradually becomes sticky. After adding 85 ml of sulfolane, change to vacuum distillation. At this time, gradually increase the reaction temperature to the final 140°C. ℃, vacuum for 7-8 hours, and the water content is 0.38%. Cool the reaction liquid to 0°C, add sodium hydroxide aqueous solution dropwise to adjust the pH=12-13, start to gradually heat up with...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More