Hallo guys,
I also prefer method in DCM.
I mixed 100g of Bromketon in 300ml DCM and slowly added 200ml of Methylamin 40%a.q. solution.
Now my question, what temperature and what time would be the best.
Last time I kept temperature at 36 - 37 degrees and reaction-time was 3hours.
But the product was extremly blue after acification.
How can I repair the relation between temperature and cooking time best.
Smaller temperature = longer reaction time?
Which temperature are not working.
Can anybody help and explain the reasons of temperature and cooking time?
Thank you a lot.
I also prefer method in DCM.
I mixed 100g of Bromketon in 300ml DCM and slowly added 200ml of Methylamin 40%a.q. solution.
Now my question, what temperature and what time would be the best.
Last time I kept temperature at 36 - 37 degrees and reaction-time was 3hours.
But the product was extremly blue after acification.
How can I repair the relation between temperature and cooking time best.
Smaller temperature = longer reaction time?
Which temperature are not working.
Can anybody help and explain the reasons of temperature and cooking time?
Thank you a lot.
- By TheVacuumGuy
experimentsciMy experience is that you can easily do it at 40 (rm temp! Use glass thermometer which goes into your mixture). DCM seems very reluctant to start actually boiling (like it has some buffer zone of sorts). If I increase temp it stubbornly keeps sitting at 40.
Either way. That relation time/temp thing is only important for those in a constant hurry. The fact that a reaction takes a certain time doesn't mean you need to stopwatch tightly. Product doesn't walk away. On 35 overnight, 25 overnight, 40 in 2 hours, 40 in 8 hours . you'll get the same output (where, imho, longer = better).
Either way. That relation time/temp thing is only important for those in a constant hurry. The fact that a reaction takes a certain time doesn't mean you need to stopwatch tightly. Product doesn't walk away. On 35 overnight, 25 overnight, 40 in 2 hours, 40 in 8 hours . you'll get the same output (where, imho, longer = better).
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- By TheVacuumGuy
TheVacuumGuyyesterday acidified, white yellowish-hue (Cream-like), started with 500ml (freebase-in-solvent) when took it from the freezer.
Acidifying, became thick, pouring aceton made volume much larger , still thick., so sended up 2000ml still quite thick creamy like substance which looks beautiful.
I decide not for adding more acetone as, a moderate thickness keeps vacuumdistill much more clean.
This morning took it from freezer. Still the same beautiful off-white color. Took it through vacuum distill, no acetone needed ecept for rinsing the beaker of leftovers.
I used the same dish as the (400g couple of reactions above), to dry.
can't see by the eye exactly, but it looks like nearly (minus a bit) as much. will report when dry.
Acidifying, became thick, pouring aceton made volume much larger , still thick., so sended up 2000ml still quite thick creamy like substance which looks beautiful.
I decide not for adding more acetone as, a moderate thickness keeps vacuumdistill much more clean.
This morning took it from freezer. Still the same beautiful off-white color. Took it through vacuum distill, no acetone needed ecept for rinsing the beaker of leftovers.
I used the same dish as the (400g couple of reactions above), to dry.
can't see by the eye exactly, but it looks like nearly (minus a bit) as much. will report when dry.
Last edited:
- By $!$
TheVacuumGuyform 1kg 2b4m 400g 4mmc powder or crystal ?? wow
i was get much year a go 880g powder 820g crystal on dcm now for me 600g crystal is better who i do all my work in 2h crystal i made on now the same day.All info how to made u have on forum if u know somting about chemistry
i was get much year a go 880g powder 820g crystal on dcm now for me 600g crystal is better who i do all my work in 2h crystal i made on now the same day.All info how to made u have on forum if u know somting about chemistry
- By TheVacuumGuy
$!$265,5.
The reaction I did shortly thereafter was one from 200g but used 800 dcm. This one yielded 165g. So that's around 75 percent (when accounted for some losses during crystallize). Much better than the one where used too little DCM.
So the 6 hour reaction I have to admit it didnt work as good (for future readers)
The reaction I did shortly thereafter was one from 200g but used 800 dcm. This one yielded 165g. So that's around 75 percent (when accounted for some losses during crystallize). Much better than the one where used too little DCM.
So the 6 hour reaction I have to admit it didnt work as good (for future readers)
- By $!$
TheVacuumGuy2h 40° to najlepszy sposób na dcm true.
A lot u lost when u wash it acetone much product is still on dcm when u wash it
A lot u lost when u wash it acetone much product is still on dcm when u wash it
