I tried this once and didnt have much good luck but this is what a supplier gave me! AGAIN I SOMEHOW FAILED AND HAVE NO CLUE WHY.
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!!!!DO NOT TAKE THIS AS FOR SURE ADVICE. I AM SIMPLY SHARING WHAT A SUPPLIER GAVE ME AND IT DIDNT TURN OUT GOOD THE FIRST TIME!!!!!
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The Main material 1kg Im not sure what this one is.
DMF CAS 68-12-2 3L
850g of Potassium carbonate CAS 584-08-7
5bromo-1pentene 500g
Step 1
Put the DMF into machine and start stir,then put all the main material in.Waiting about 10
minutes,put the 850g of potassium carbonate in and turn on heating,maintain heating rate
at 300-380.Turn off the heating when reaching 55 degrees.
PS:The potassium carbonate will not sink to the bottom if reacts sufficiently.
Step 2
Stir for a minute and get the bromo pentene in drop by drop slowly.At this time
the temperature will slowly rise.
Step 3
When the bromopentene are fully add in. Watch the temperature in machine and turn on
heating.Keeping the temperature at 85-90 degrees for 3 to 4 hours.
Step 4
Turn off the heating after 3 to 4 hours and waiting cool down to roomS temperature.If you
want to cool it quickly,fill it with ice cubes.
Step 5
The potassium carbonate needs to be completely washed off.Otherwise the purity of finished
product will be reduced.Potassium carbonate is soluble in water.Neutral,indicating that all
the potassium carbonate already has been washed off by water.
Prepare ice water(4-5 times of DMF)in a container,the ice water means crushed ice with
low temperature water under 20 degrees.Put the cooled reaction liquid into ice water
slowly.There will be white or little yellow color being start separated out.
30 minutes after putting all the cooled reaction liquid into ice water,stir slowly by speed of
100 rolls per 2 minutes.Repeat this process three times until the wash water's PH is 7 or
under 7,then filter the solid.The white powder filter cake is the finished product.
Step 6
Dry the solid,it can be air-dried at natural temperature
William Is helping me finish this kit. I have all of his instuctions and a fresh kit to start with. I love this forum because everyone is so supportive. Thank You very much guys. Hopefully i can donate $100 usd very soon.
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