Amide chromatographic stationary phase and preparation method thereof
A chromatographic stationary phase and amide-based technology, applied in the field of new amide stationary phases, can solve the problems of poor reproducibility and short service life, and achieve the effects of good separation selectivity, wide application range and novel structure
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0023] Under the protection of nitrogen, add 500mL of toluene, 30mL of mercaptopropyltrimethoxysilane and 40g of microspherical silica gel dried at 120°C for 18 hours in a 1000mL flask, react at 110°C for 16 hours, filter, and wash with dichloromethane, methanol in turn , water and methanol, and the resulting solid was dried in a vacuum oven at 40°C for 12 hours to obtain mercaptopropyl silica gel.
[0024] Add 40g of mercapto silica gel, 160mL of N,N-dimethylformamide and 18g of iodoacetamide into a 250mL flask, then add 8mL of triethylamine, react at 60°C for 16 hours, filter, and wash with methanol, water, and methanol in sequence After washing, the obtained solid was dried in a vacuum oven at 60° C. for 12 hours to obtain amido silica gel.
[0025] Add 40g of amido silica gel and 300mL of 10% hydrogen peroxide solution into a 500mL flask, stir at room temperature for 8 hours, wash with water and methanol in turn, and dry the obtained solid in a vacuum oven at 60°C for 8 ho...
Embodiment 2
[0028] Under nitrogen protection, add 80mL of acetonitrile, 10mL of mercaptopropyltrimethoxysilane and 20g of microspherical silica gel dried at 120°C for 18 hours into a 200mL flask, react at 80°C for 24 hours, filter, and wash with dichloromethane, methanol in turn , water and methanol, and the resulting solid was dried in a vacuum oven at 60°C for 12 hours to obtain mercaptopropyl silica gel.
[0029] Add 12g of mercapto silica gel, 50mL of N,N-dimethylformamide and 5g of acrylamide into a 150mL flask, then add 2mL of diisopropylethylamine, react at 80°C for 12 hours, filter, and wash with methanol, water, After washing with methanol, the resulting solid was dried in a vacuum oven at 60° C. for 12 hours to obtain amido silica gel.
[0030] Add 12g of amido silica gel and 150mL of 20% hydrogen peroxide solution into a 300mL flask, stir at room temperature for 8 hours, wash with water and methanol in turn, and dry the obtained solid in a vacuum oven at 60°C for 8 hours to obt...
Embodiment 3
[0033] Under the protection of nitrogen, add 500mL of toluene, 30mL of mercaptopropyltrimethoxysilane and 40g of microspherical silica gel dried at 120°C for 18 hours in a 1000mL flask, react at 110°C for 16 hours, filter, and wash with dichloromethane, methanol in turn , water and methanol, and the resulting solid was dried in a vacuum oven at 40°C for 12 hours to obtain mercaptopropyl silica gel.
[0034] Add 40g of mercapto silica gel, 160mL of N,N-dimethylformamide and 18g of iodopropionamide into a 250mL flask, then add 8mL of triethylamine, react at 60°C for 16 hours, filter, and wash with methanol, water, methanol After washing, the obtained solid was dried in a vacuum oven at 60° C. for 12 hours to obtain amido silica gel.
[0035] Add 40g of amido silica gel and 300mL of 10% hydrogen peroxide solution into a 500mL flask, stir at room temperature for 8 hours, wash with water and methanol in turn, and dry the obtained solid in a vacuum oven at 60°C for 8 hours to obtain...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More