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Synthesis of Euphor via bromination of safrole

Joni

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Eufor - through the bromination of safrole.

200 ml of ice-cold acetic acid is poured into a champagne bottle. After cooling, slowly stirring, 200 ml of 48% bromide to-you are added dropwise. After cooling, slowly stirring, 100 g of safrole* is added. After that, the bottle is tightly stoppered. The bottle must be shaken regularly. After about 12 hours, the two layers will combine into one fraction of red. Then leave the bottle for 24 hours.

After carefully open the cork. Pour the product into a two-liter bowl, on the bottom of which you should first put 500 g of crushed ice. When the ice begins to melt, the red liquid will begin to separate (precipitate or an oily fraction forms from below). the upper fraction is no longer needed. and the lower one is washed with a solution of sodium carbonate to remove bromide from it. A sign of the readiness of this stage is when the substance stops reacting with soda.

Next, you need to remove the ether fractions from the Islands. To do this, the drink is placed in a flask and closed with a stopper, into which a glass tube is embedded in the middle. the flask is placed in a water bath. Boiling is stopped when about 200 g remains.
The yield of bromsafrole is about 100%
In a beaker, 200 ml of 28% ammonia solution or the same amount of 40% methylamine solution is added to 50 g of bromsafrole, and isopropyl alcohol is poured in slowly stirring until a homogeneous solution begins to form.

Next, the mixture is poured into a "stainless steel" cylinder, tightly and hermetically screwed. Then the cylinder is placed in a container with oil heated to 130 C. and kept at this temperature for about 3 hours. When the cylinder has cooled down to t 50 - 60 C, remove it and cool it under cold water and unscrew the cap. Next, put it on a very low heat to remove excess isopropyl alcohol and ammonia (or methylamine). It should be removed from the fire when the intensity of evaporation decreases. After that, concentrated hydrochloric acid should be added until the pH level approaches 3.

Purification follows: add 200 - 300 ml of diethyl ether and carefully extract. There will be division into factions. The upper fraction contains about 20 g of unreacted matter (it can be reused). Separate it from the bottom and save until the next time. For a more thorough purification of the product, the resulting lower fraction is made alkaline with an aqueous solution of KOH and extracted with two portions of diethyl ether, 100-150 ml each. Then the ether fraction is separated and distilled through a direct refrigerator, preferably with a reflux condenser at a temperature of 150-160C
The yield should be about 20 g of a light yellow transparent oil.

You can do without acetic acid: 5.3 g of safrole are cooled and mixed drop by drop with 21 g of 48% HBr at 0C. The mixture is kept at zero temperature to flow. 14 hours. The mixture was then poured onto crushed ice and extracted with two 30 ml portions of ether. The ether is dried with baking soda and distilled off. Yield 97%.
With HI, the yield is about the same, but the reaction is faster.
When using HCl, the reaction is slower, the yield is lower. Due to the lengthening of the reaction time, the risk of polymerization increases, but this can be easily prevented by dissolving safrole in benzene. Pace. The boiling point of chlorsafrole should be between those of safrole and bromosafrole.
 
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