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ASheSChem

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can we use 80% acid acetic or only glacial ?
 

ASheSChem

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Ok, Thanks !
 

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When using aqueous acetic acid, you will most likely have to use some alcohol all at once to dissolve the water, benzaldehyde, and nitroethane together
William Dampier
like 100 ml benzaldehyde, 100 ml nitroethane, 20 ml acetic acid 80%, 5ml isopropanol and 10ml (or 20ml?) cyclohexilamine in 1 L flask and reflux ?
 
Last edited:

WillD

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like 100 ml benzaldehyde, 100 ml nitroethane, 20 ml acetic acid 80%, 5ml isopropanol and 10ml (or 20ml?) cyclohexilamine in 1 L flask and reflux ?
ASheSChemMix everything and add isopropanol until the mixture becomes homogeneous. After add a little more for boils and start the reaction.
 

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Thank you very much I will also try this technique, we will see if I have a bigger harvest
 

ASheSChem

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i have tried ! and it's my actual yield record haha thanks !!

55gr benzaldehyde
40gr nitroethane
10ml acid acetic 80°
3ml isopropanol 99.9%
10ml cyclohexylamine

2:20 p.m. - start of mixing, hotplate at maximum
2:28 p.m. - seems homogeneous to me, with small oily reflections but if I don't see any bubbles
2:32 p.m. - I see bubbles forming in the liquid
2:33 p.m. - I lower the temperature (as I usually do) and turn on the mixer, strong for a few minutes then reduce it a little
6:00 p.m. - I stop and let it cool
7:00 p.m. - add 100ml of isopropanol, mix well (magnetic) and freeze.

09:00 a.m. - I start to filter by gravity the frozen product by mixing regularly
12:00 p.m. - transfer to a pyrex dish for the end of drying (in an incubator)
8:30 p.m. - weighed and transferred to the fridge, 67.7gr. - (71.11%)

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MCAIjwp92x
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MlwHuK3PpI
 

flyhigh

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i have tried ! and it's my actual yield record haha thanks !!

55gr benzaldehyde
40gr nitroethane
10ml acid acetic 80°
3ml isopropanol 99.9%
10ml cyclohexylamine

2:20 p.m. - start of mixing, hotplate at maximum
2:28 p.m. - seems homogeneous to me, with small oily reflections but if I don't see any bubbles
2:32 p.m. - I see bubbles forming in the liquid
2:33 p.m. - I lower the temperature (as I usually do) and turn on the mixer, strong for a few minutes then reduce it a little
6:00 p.m. - I stop and let it cool
7:00 p.m. - add 100ml of isopropanol, mix well (magnetic) and freeze.

09:00 a.m. - I start to filter by gravity the frozen product by mixing regularly
12:00 p.m. - transfer to a pyrex dish for the end of drying (in an incubator)
8:30 p.m. - weighed and transferred to the fridge, 67.7gr. - (71.11%)

ASheSChemwith same quantities can you suggest what quantity of n-butlyamine to be used ? instead of cyclohexylamine ?
 

flyhigh

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i have tried ! and it's my actual yield record haha thanks !!

55gr benzaldehyde
40gr nitroethane
10ml acid acetic 80°
3ml isopropanol 99.9%
10ml cyclohexylamine

2:20 p.m. - start of mixing, hotplate at maximum
2:28 p.m. - seems homogeneous to me, with small oily reflections but if I don't see any bubbles
2:32 p.m. - I see bubbles forming in the liquid
2:33 p.m. - I lower the temperature (as I usually do) and turn on the mixer, strong for a few minutes then reduce it a little
6:00 p.m. - I stop and let it cool
7:00 p.m. - add 100ml of isopropanol, mix well (magnetic) and freeze.

09:00 a.m. - I start to filter by gravity the frozen product by mixing regularly
12:00 p.m. - transfer to a pyrex dish for the end of drying (in an incubator)
8:30 p.m. - weighed and transferred to the fridge, 67.7gr. - (71.11%)

ASheSChemis it 55grams benzaldehyde or 55ml ? coz density is 1.04gm/L and in the picture your flask size is 200ml , so im guessing it must be 55ml
please suggest
 

ASheSChem

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Second try with acid acetic :

55.4gr benzaldehyde
40.1gr nitroethane
11ml acid acetic 80°
5ml isopropanol 99.9%
10ml cyclohexylamine

same procedure, just waiting a little more little bubbles (a lot on my maggnetic stirrer) at the bigining

weighed and transferred to the fridge, 69.6gr. - (72.88%)
 

WillD

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Did you leave a filtrate in the freezer?
 

ASheSChem

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what do you mean, re-freeze the liquid filtered another time?
 

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at first I threw everything away... now I try to refreeze for the experiment; and this gives new crystals... sometimes even very long

but I don't know if it's a good product, I separate the refreezing from the rest of the harvest

View attachment 4664
ASheSChemThe crystals look good. In the first crystallizations, there was little alcohol, so the sediment fell out densely.
 

yin-yang

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Can I use this for as a catalyst? N- is same as 1- right?

1-Butylamine
CAS no: 109-73-9

I know there are some isomers so wanna make sure this is the right one.
 

yin-yang

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Also, I heard you can recover N-Butylamine and re-use it again. How to do that exacly?
 

yin-yang

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quite close to isopropyl bp- 82.5. should i use fractional destination or regular can get job done ?
 
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