Have any of your friends tried this method ???
Materials
10.8 g phenylhydrazine
10.6 g chlorobutyric aldehyde (4-chlorobutanal)
ethyl alcohol
80% ethanol
ether
sodium sulfate
benzene
caustic soda
0.1 N hydrochloric acid
Description of the method
Solutions of 10.8 g (0.1 mol) of phenylhydrazine in 100 ml of 80% ethanol and 10.6 g (0.1 mol) of freshly prepared chlorobutyric aldehyde in 200 ml of ethyl alcohol and boil in a water bath for 6 hours. The solvent is then distilled off in a water-jet pump vacuum, dry total tryptamine hydrochloride is dissolved in 100 ml of 0.1 N hydrochloric acid solution and neutral impurities are extracted with 45 ml of ether (3 x 15 ml). The aqueous layer is alkalized with caustic soda and the released tryptamine is extracted with benzene (3 times 30 ml). The benzene extract is filtered, dried over calcined sodium sulfate, the solvent is distilled off in a water-jet pump vacuum, and the oily extract is completely distilled in a stream of dry nitrogen, collecting a fraction boiling at 185-188 ° (0.5 mm Hg). The resulting yellowish thick oil solidifies quickly. If necessary, recrystallize from 50 ml of a mixture of petroleum ether and benzene 3:1.
Yield 11.2 g (70.0% of theory).
Reaction mechanism
Materials
10.8 g phenylhydrazine
10.6 g chlorobutyric aldehyde (4-chlorobutanal)
ethyl alcohol
80% ethanol
ether
sodium sulfate
benzene
caustic soda
0.1 N hydrochloric acid
Description of the method
Solutions of 10.8 g (0.1 mol) of phenylhydrazine in 100 ml of 80% ethanol and 10.6 g (0.1 mol) of freshly prepared chlorobutyric aldehyde in 200 ml of ethyl alcohol and boil in a water bath for 6 hours. The solvent is then distilled off in a water-jet pump vacuum, dry total tryptamine hydrochloride is dissolved in 100 ml of 0.1 N hydrochloric acid solution and neutral impurities are extracted with 45 ml of ether (3 x 15 ml). The aqueous layer is alkalized with caustic soda and the released tryptamine is extracted with benzene (3 times 30 ml). The benzene extract is filtered, dried over calcined sodium sulfate, the solvent is distilled off in a water-jet pump vacuum, and the oily extract is completely distilled in a stream of dry nitrogen, collecting a fraction boiling at 185-188 ° (0.5 mm Hg). The resulting yellowish thick oil solidifies quickly. If necessary, recrystallize from 50 ml of a mixture of petroleum ether and benzene 3:1.
Yield 11.2 g (70.0% of theory).
Reaction mechanism
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