Question Is it possible to convert nitromethane to nitroethane?
- Thread starter senseiFreu
- Start date
-
- Tags
- ampheamine nitroethane
this would be the most resource wasteful challenge for a very bored but yet bright chemist and it is rather fundamental science than applied so it will only eventually prove it can be done but asking the yield would be an insult and you will face an explanation of the word fundamental in science from a potentially pissed off competent chemist...
`` Preparation of Nitroethane
by Gerard Desseigne & Henri Giral
The reaction flask is charged with:
26.5 g (0.0625 * 3moles) of tech grade K2CO3 dissolved in 137 g of water
320 g of 97% tech sodium nitrite
6 ml of cetyl-oleic alcohol or oleic alcoholm(antifoaming agent)
Vol of the mixture is about 420 mls
The mixture is heated on a bath at 130C with stirring. The addition funnel
is charged with 750 ml of an aqueous solution of 444 g (3moles) sodium ethyl
sulfate. The solution is added to the reaction mixture during 50-60 mins at a
suitable rate to keep the reaction mixture at 125-130C, with vigorous
stirring.
The distillation of the nitroethane begins when the addition is started.
When addition of NaEtSO4 is complete 100 mls of water is added during 10 mins.
The distillate separates into 2 layers. Can be distilled at 760mmHg with a distillation column. Distillation starts at 30C. All below 74C is discarded. Temp should settle
at 87C & distillation is stopped at 99.8C.
Yield of nitroethane:96 g (1.28 moles), 42.6% based on NaEtSO4
I tried both the dry distillation and the one described above (solutions mixed). Got less than half a ml each time, but then again I started with 2g each of nitrite and Na-ethylsulfate.
72 grams of NaEtSO4 are sitting in my dessicator at this moment. Let's see how it goes next time. BTW the EtONO danger is new to me. Oh and the NaEtSO4 was made from sulfuric, everclear, lime and soda as is described in Rhodium's "nitroalkane preparation FAQ". ``
I found a larger-scale synthesis as follows. Can I use different foam inhibitors other than cetyl oleic alcohol or oleic alcohol used here?
by Gerard Desseigne & Henri Giral
The reaction flask is charged with:
26.5 g (0.0625 * 3moles) of tech grade K2CO3 dissolved in 137 g of water
320 g of 97% tech sodium nitrite
6 ml of cetyl-oleic alcohol or oleic alcoholm(antifoaming agent)
Vol of the mixture is about 420 mls
The mixture is heated on a bath at 130C with stirring. The addition funnel
is charged with 750 ml of an aqueous solution of 444 g (3moles) sodium ethyl
sulfate. The solution is added to the reaction mixture during 50-60 mins at a
suitable rate to keep the reaction mixture at 125-130C, with vigorous
stirring.
The distillation of the nitroethane begins when the addition is started.
When addition of NaEtSO4 is complete 100 mls of water is added during 10 mins.
The distillate separates into 2 layers. Can be distilled at 760mmHg with a distillation column. Distillation starts at 30C. All below 74C is discarded. Temp should settle
at 87C & distillation is stopped at 99.8C.
Yield of nitroethane:96 g (1.28 moles), 42.6% based on NaEtSO4
I tried both the dry distillation and the one described above (solutions mixed). Got less than half a ml each time, but then again I started with 2g each of nitrite and Na-ethylsulfate.
72 grams of NaEtSO4 are sitting in my dessicator at this moment. Let's see how it goes next time. BTW the EtONO danger is new to me. Oh and the NaEtSO4 was made from sulfuric, everclear, lime and soda as is described in Rhodium's "nitroalkane preparation FAQ". ``
I found a larger-scale synthesis as follows. Can I use different foam inhibitors other than cetyl oleic alcohol or oleic alcohol used here?
