i am using three neck round bottom flask on the heating mental at 250oC, usually i add precursor, oleylamine, surfactant and reducing agent at the same time and then i rise the temperature to 250oC but i can not get any product.
It has to do with the nature of precursors and reducing agent. Check the boiling temperature of reducing agent, which should be lower than the reaction temperature. Also it can help if you try higher reaction temperatures than 250C. Sufactants like oleic acid tend to increase the precursor decomposition temperature. Please browse some of my recent publications to obtain detailed information.
I suggest you try this reaction at lower temperature.. If possible use tri-sodium citrate or any member from polysaccharides.
Good luck
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