This synthesis is describe in book "Preparation and elements of organic synthesis" by Jerzy T. Wróblewski.
It was transleted by me from Polisch to Englisch.
1. Obtaining IUPAC
nedded:
three-necked flask (250 cm^3)
stirrer, dropper, reflux condenser
thermometer
45g concentrated sulfuric acid
40g acetonitrile
23,6g Allylbenzene (phenylpropene)
400 cm^3 - 15% sodium hydroxide solution
A) In three necked flask with 250 cm^3 capacity stocked with stirrer, dropping funnel and reflux condenser, 45g of concentrated sulfuric acid was placed and when stiring was cooled to 5 degree Celsius. Then carefully drop by drop 40g (1 mole) of acetonitrile was added in way that solution remains still at 5-10 degree Celsius next 23.6g (0.2 mole) of allylbenzene was added. While stirring a cool bath is removed and dropper is changed to thermometer. A turbid orange coloured suspension slowly after some time undergous homogenization and darkens due to self increasing temperature.
At the beginning tempretaure slowly raises to 50 degree Celsius then a bit faster to 80 degree and then slowly starts to cool. After cooling everything is carefully poured into 400 cm3 15% sodium hydroxide solution.
Separated light yellow oil is then let stayed for a few hours to solidification. The precipitated is filtered off in reduced pressure and is washed with water and dried off on air.
We got a raw
IUPAC with efficency of 40% (14g).
It can be purified by destilation ( boiling temp. 180-185 degree Celsius / 17 hPa) or by crystalization with n-hexane (t.t. 88-89 degree)
2. obtaining 1-phenyl-2-aminopropane
Nedded:
9.2g IUPAC
100 cm^3 of 15% hydrochloric acid
Benzene
sodium hydroxide
Separating funnel
Reflux condenser
B) Under the reflux condenser 9.2g (0.047mole) of IUPAC and 100 cm^3 of 15% hydrochloric acid solution is being heated at boiling temperature for an 1 hour.
After being cooled everything is being placed in separatory funnel and washed with benzene. The aqueous layer is carefully alkalized with sodium hydroxide, then saperated oil is extracted with benzene and dreid with anhydrous sodium sulfate, next trickled and benzene is distiled off.
Next collects the boiling fraction in range of 205-210 degree Celsius. 1-phenyl-2-aminopropane is gathered at eficiency of 67% (7g). t.t. the benzoyl derivative 134-135 degree Celsius.
It was transleted by me from Polisch to Englisch.
1. Obtaining IUPAC
nedded:
three-necked flask (250 cm^3)
stirrer, dropper, reflux condenser
thermometer
45g concentrated sulfuric acid
40g acetonitrile
23,6g Allylbenzene (phenylpropene)
400 cm^3 - 15% sodium hydroxide solution
A) In three necked flask with 250 cm^3 capacity stocked with stirrer, dropping funnel and reflux condenser, 45g of concentrated sulfuric acid was placed and when stiring was cooled to 5 degree Celsius. Then carefully drop by drop 40g (1 mole) of acetonitrile was added in way that solution remains still at 5-10 degree Celsius next 23.6g (0.2 mole) of allylbenzene was added. While stirring a cool bath is removed and dropper is changed to thermometer. A turbid orange coloured suspension slowly after some time undergous homogenization and darkens due to self increasing temperature.
At the beginning tempretaure slowly raises to 50 degree Celsius then a bit faster to 80 degree and then slowly starts to cool. After cooling everything is carefully poured into 400 cm3 15% sodium hydroxide solution.
Separated light yellow oil is then let stayed for a few hours to solidification. The precipitated is filtered off in reduced pressure and is washed with water and dried off on air.
We got a raw
IUPAC with efficency of 40% (14g).
It can be purified by destilation ( boiling temp. 180-185 degree Celsius / 17 hPa) or by crystalization with n-hexane (t.t. 88-89 degree)
2. obtaining 1-phenyl-2-aminopropane
Nedded:
9.2g IUPAC
100 cm^3 of 15% hydrochloric acid
Benzene
sodium hydroxide
Separating funnel
Reflux condenser
B) Under the reflux condenser 9.2g (0.047mole) of IUPAC and 100 cm^3 of 15% hydrochloric acid solution is being heated at boiling temperature for an 1 hour.
After being cooled everything is being placed in separatory funnel and washed with benzene. The aqueous layer is carefully alkalized with sodium hydroxide, then saperated oil is extracted with benzene and dreid with anhydrous sodium sulfate, next trickled and benzene is distiled off.
Next collects the boiling fraction in range of 205-210 degree Celsius. 1-phenyl-2-aminopropane is gathered at eficiency of 67% (7g). t.t. the benzoyl derivative 134-135 degree Celsius.
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