ChemicalBook CAS DataBase List 4-Nitrophenethylamine hydrochloride

4-Nitrophenethylamine hydrochloride synthesis

7synthesis methods

Product Name:4-Nitrophenethylamine hydrochloride
CAS Number:29968-78-3
Molecular formula:C8H11ClN2O2
Molecular Weight:202.64

The preparation of 4-Nitrophenethylamine hydrochloride is as follows:Ten mL of 2M HCl was then added in a one-pot fashion, and, in all cases but threonine, the reaction vessel was heated to 190°Cover 5 min with stirring and then allowed to cool. In the case of the temperature-sensitive threonine, soxhlet extraction with toluene was performed at 80°C to remove R-carvone from the reaction mixture. The aqueous reaction mixture was washed three times with 25 mL of ether, and then water solvent was distilled off from the hydrochloride salt. The hydrochloride salt was transferred to a vacuum oven and dried overnight at 150 °C and 10 Torr.

29968-78-3(1).png

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Yield:29968-78-3 84.7%

Reaction Conditions:

with hydrogenchloride in ethanol;water; pH=1; for 20 h;Reflux;Large scale;

Steps:

2

140 kg of intermediate 2 was dissolved in 190 kg of ethanol in a reaction kettle, and dissolved under constant stirring, the pH was adjusted to 1 with 2mol/L hydrochloric acid, and the reaction solution was heated to 80° C for 20 hours, after the reaction was completed, the reaction solution was cooled to room temperature and solids precipitated, the crude product was recrystallized from methanol to give 116 Kg of finished p-nitrophenylethylamine hydrochloride after filtration and centrifugation, the final product purity was 99.6%, and the yield of this step was 84.7%.

References:

CN107759477,2018,A Location in patent:Paragraph 0063