A kind of preparation method of isopulegol
A technology of isopulegol and calixarene, which is applied in the field of preparation of isopulegol, can solve the problems of high raw material cost, harsh operating conditions, and a large amount of waste solid waste water, etc., to improve conversion rate and selectivity, and increase yield , the effect of avoiding emissions
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0033] To a 100ml four-neck flask equipped with a stirring, reflux tube, thermometer sleeve and constant pressure dropping funnel, add 6g of commercially available anhydrous zinc bromide catalyst (analytical grade, Sinopharm Chemicals Co., Ltd.) and 35ml of toluene. in N 2 Cool down to 0°C under protection, drop 10g of a mixture of 98.92% racemic citronellal and 10g toluene from the constant pressure dropping funnel, add the mixture for 2 hours, keep the temperature for reaction after the citronellal is added dropwise Sampling gas phase detection after 5 hours, the transformation rate of citronellal is 98.24%, the selectivity of isopulegol is 90.24%, neo-isopulegol 2.15%, different-isopulegol 3.56%, citronellal dimerization Body 2.98%. Add 10 ml of 0.05 mol / L HBr aqueous solution to the reaction solution for stratification, recover toluene from the oil phase and rectify to obtain 7.95 g of isopulegol product, the content of isopulegol is 94.29%. The yield of isopulegol was 7...
Embodiment 2
[0035] In the 100ml four-neck flask equipped with stirring, reflux tube, thermometer sleeve and constant pressure dropping funnel, add 6g of zinc bromide catalyst and 55ml of toluene, heat to toluene reflux for 1 hour, and take 20ml of toluene, take The refluxed toluene was tested with a moisture titrator, and the water content was 0.015%. in N 2 Cool to 0°C under protection, add dropwise a mixture of 10g of 98.92% racemic citronellal and 10g of toluene from the constant pressure dropping funnel, dropwise for 2 hours, keep warm for 5 hours after adding citronellal After the sampling gas phase detection, the transformation rate of citronellal is 98.24%, the selectivity of isopulegol is 92.54%, neo-isopulegol 2.05%, different-isopulegol 3.36%, citronellal dimer 0.98% %. Add 10 ml of 0.05 mol / L HBr aqueous solution to the reaction solution for stratification, recover the toluene from the oil phase and rectify to obtain 9.18 g of isopulegol product, the content of isopulegol is ...
Embodiment 3
[0037] Add 6g of ZnBr 2 And the toluene of 55ml, be heated to toluene reflux 1 hour, and take out the toluene of 20ml, get back flowing toluene and detect with water content titrator, water content 0.018%. in N 2Cool to 5°C under protection, add 0.1g tert-butylcalix[6]arene, add dropwise 10g content of 99.15% enantiomeric excess ee% D-citronellal and 10g from constant pressure dropping funnel The mixture of toluene, the time of dropping for 1 hour, after the citronellal was added dropwise and then incubated for 2 hours, the gas phase detection and chiral detection were sampled, the conversion rate of citronellal was 99.72%, and the selectivity of isopulegol was 97.6% %, neo-isopulegol 0.56%, iso-isopulegol 1.34%, citronellal dimer 0.4%. The ee value of isopulegol is 79.8%. Add 10 ml of 0.05 mol / l HBr aqueous solution to the reaction solution for stratification, recover toluene from the oil phase and rectify to obtain 9.77 g of isopulegol product, the content of isopulegol i...
PUM
| Property | Measurement | Unit |
|---|---|---|
| water content | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More