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Harm Reduction Resources / Re: Tiny write up and big ambitions
« Last post by Samppa092 on July 07, 2023, 12:29:56 AM »Hey bees! Im extremely happy right now and would like to share my now-finished project (alt for Samppa0920):
Chlorobutanol
1. 50ml acetone + 1,6l sodium hypochlorite (10%) -> chloroform (around ~30ml)
2. 90ml acetone + 10ml chloroform (1g KOH catalyst) -> chlorobutanol (~10g)
1. I started off with the chloroform by adding the acetone to an ice cold bucket of hypochlorite (adding ice whenever necessary to keep cool)
The bottom aqueous layer (chloroform) was poured in a container with a layer of around ~5ml of water remaining on top (pic while in progress - chloroform.jpeg)
2. The acetone was cooled until chilly in a freezer and 10ml of chloroform was added to it with 1g of KOH to catalyse the reaction. (30min into it - acetone+koh+chloroform.jpeg)
The reaction was given 2 hours to with the occasional check-up and stirring, after which the solution was heated in a water bath at 85°c until
the solution seemed ok (I tried to smell for acetone & chloroform, and feel if any cold-feeling, but hot gas was coming out).
Afterwards the hot solution was poured into ice-cold water and the liquid chlorobutanol that didn't crystallize much at all was poured onto a
drying tray. (after dry - chlorobutanol.jpeg
Notes:
-I had no idea on the quantities of reactants to use, so I resorted to calculating them through NileRed's video on chlorobutanol (Making an old hypnotic sedative and preservative). I feel as if the correct amounts were used, since the amount of chloroform made was enough not to warrant the need to optimize the reaction further.
-The chloroform was not "cleaned", as it was simply collected out of the bucket after mixing the acetone&hypochlorite.
-While the acetone and chloroform were reacting, they were forgotten to be kept chilly for a short bit (5-15min?), slight warmness was felt on the side of the flask, after which the reaction was placed to continue in the freezer.
-KOH wasn't filtered out at any point, so the final product has 1g of KOH in it. The pH of the end product was tested to be 6, which I think is due to the KOH left in it. It is noted on pubchem, that chlorobutanol is stable for many months at a pH 5 solution, so eitherway the final product seems fine.
-The chlorobutanol didn't crystallize (I guess due to the KOH), next time I'll remember to filter it out first before boiling the solution.
Chlorobutanol
1. 50ml acetone + 1,6l sodium hypochlorite (10%) -> chloroform (around ~30ml)
2. 90ml acetone + 10ml chloroform (1g KOH catalyst) -> chlorobutanol (~10g)
1. I started off with the chloroform by adding the acetone to an ice cold bucket of hypochlorite (adding ice whenever necessary to keep cool)
The bottom aqueous layer (chloroform) was poured in a container with a layer of around ~5ml of water remaining on top (pic while in progress - chloroform.jpeg)
2. The acetone was cooled until chilly in a freezer and 10ml of chloroform was added to it with 1g of KOH to catalyse the reaction. (30min into it - acetone+koh+chloroform.jpeg)
The reaction was given 2 hours to with the occasional check-up and stirring, after which the solution was heated in a water bath at 85°c until
the solution seemed ok (I tried to smell for acetone & chloroform, and feel if any cold-feeling, but hot gas was coming out).
Afterwards the hot solution was poured into ice-cold water and the liquid chlorobutanol that didn't crystallize much at all was poured onto a
drying tray. (after dry - chlorobutanol.jpeg
Notes:
-I had no idea on the quantities of reactants to use, so I resorted to calculating them through NileRed's video on chlorobutanol (Making an old hypnotic sedative and preservative). I feel as if the correct amounts were used, since the amount of chloroform made was enough not to warrant the need to optimize the reaction further.
-The chloroform was not "cleaned", as it was simply collected out of the bucket after mixing the acetone&hypochlorite.
-While the acetone and chloroform were reacting, they were forgotten to be kept chilly for a short bit (5-15min?), slight warmness was felt on the side of the flask, after which the reaction was placed to continue in the freezer.
-KOH wasn't filtered out at any point, so the final product has 1g of KOH in it. The pH of the end product was tested to be 6, which I think is due to the KOH left in it. It is noted on pubchem, that chlorobutanol is stable for many months at a pH 5 solution, so eitherway the final product seems fine.
-The chlorobutanol didn't crystallize (I guess due to the KOH), next time I'll remember to filter it out first before boiling the solution.
) and veteran bees alike! I hope to someday be able to guide someone such as myself to the start of their journey to self-reliance – Long live the hive!