Chelating agent and preparation method and application thereof
A chelating agent and compound technology, applied in the field of green chemistry, can solve the problems of complex preparation methods, low extraction efficiency, secondary pollution, etc., and achieve the effect of easy-to-obtain raw materials, high yield, and less reaction by-products
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0047] At room temperature, add 5 mL of acetonitrile solution containing 0.05 mmol of bisphosphorimide sodium salt into a 50 mL round bottom flask, and dropwise add 10 mL of acetonitrile solution containing 0.20 mmol of iodoisoctane and 0.005 mmol of tetrabutylammonium bromide , continue to stir, and stop the reaction after 10 hours of reaction; the reactant is vacuum distilled to remove acetonitrile, and the distillation residue is dissolved in 30 mL of dichloromethane, and washed three times with deionized water (about 30 mL of deionized water each time). The organic layer was collected and dried with anhydrous sodium sulfate, filtered to remove sodium sulfate, the organic solution was collected, vacuum distilled, and the remaining mixture was subjected to flash silica gel chromatography (the eluent was a mixed solution of ethyl acetate and petroleum ether with a volume ratio of 1:7). ) purification, that is, 28 mg of bis-(O, O-diisooctylphosphoryl)imide was obtained as a lig...
Embodiment 2
[0049] At room temperature, 5 mL of acetonitrile solution containing 0.05 mmol of bisphosphorimide sodium salt was added to a 50 mL round bottom flask, and 5 mL of 0.20 mmol (3-chloropropyl) trimethylsilane and 0.0003 mmol of 15-crown -5 acetonitrile solution, keep stirring, and stop the reaction after 8 hours of reaction; the reactant is vacuum distilled to remove acetonitrile, and the distillation residue is dissolved in 20 mL of dichloromethane, and washed three times with deionized water (about 20 mL of deionized water each time). The organic layer was collected and dried with anhydrous sodium sulfate, filtered to remove sodium sulfate, the organic solution was collected, vacuum distilled, and the remaining mixture was subjected to flash silica gel chromatography (the eluent was a mixed solution of ethyl acetate and petroleum ether with a volume ratio of 1:9). ) purification, that is, 26.6 mg of bis-[O, O-bis(3-trimethylsilyl-propyl) phosphoryl]imide was obtained as a brown...
Embodiment 3
[0051] At room temperature, 5 mL of acetonitrile solution containing 0.05 mmol of bisphosphorimide sodium salt was added to a 50 mL round bottom flask, and 5 mL of 0.20 mmol (2R, 3R, 4S, 5R, 6R)-2-(acetoxy methyl)-6-(3-bromopropyl)tetrahydro-2H-pyran-3,4,5-triacetate and 0.0003mmol 15-crown-5 acetonitrile solution, stirring continuously, after 10h of reaction Stop the reaction; remove acetonitrile from the reactant by vacuum distillation, and dissolve the distillation residue in 20 mL of dichloromethane, and wash with deionized water three times (about 20 mL of deionized water each time). The organic layer was collected and dried with anhydrous sodium sulfate, sodium sulfate was removed by filtration, the organic solution was collected and vacuum distilled, and the remaining mixture was subjected to flash silica gel chromatography (the eluent was a mixed solution of ethyl acetate and n-hexane with a volume ratio of 1:9). ) purification to obtain bis-[O, O-bis(3-propyl-peracety...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More