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so, my experience is,
100g 2b3c
300dcm
200methylamin40% aqua
3 hours stirring
I use a sealed glas 1,8l, put foil between lid and glass so that nothing smells or gas escapes.
After reaction took place
2 times washing with dest.water
1 time extract water phase with dcm
put into rm,
add same amount fresh water into rm
put on magnetic stirrer
acidificaction drop by drop till ph6, about 50-55ml HCI,
after that take the water layer,evaporate , let it crystallize, takes some time
opt. rotovap till 50% of the water is gone, then air drop
ethylacetat is possible, takes only 20 min, no heating necessary, rest same prosedure like with dcm
100g 2b3c
300dcm
200methylamin40% aqua
3 hours stirring
I use a sealed glas 1,8l, put foil between lid and glass so that nothing smells or gas escapes.
After reaction took place
2 times washing with dest.water
1 time extract water phase with dcm
put into rm,
add same amount fresh water into rm
put on magnetic stirrer
acidificaction drop by drop till ph6, about 50-55ml HCI,
after that take the water layer,evaporate , let it crystallize, takes some time
opt. rotovap till 50% of the water is gone, then air drop
ethylacetat is possible, takes only 20 min, no heating necessary, rest same prosedure like with dcm
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Hi I'm very glad you are sharing your experience I have a few questions
What is the efficiency of this method ?
Is it possible to transfer it to plastic barrels to scale up to kilograms of finished product if so how to do it ?
For the help received, I will be happy to repay you when everything at my place starts greetings
What is the efficiency of this method ?
Is it possible to transfer it to plastic barrels to scale up to kilograms of finished product if so how to do it ?
For the help received, I will be happy to repay you when everything at my place starts greetings
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