In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-(4-Fluorophenoxy)ethylamine, other downstream synthetic routes, hurry up and to see.
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2-(4-Fluorophenoxy)ethylamine (5A-1) in hydrochloride form is dissolved in wa- ter and basified with 1N sodium hydroxide (NaOH) to basic pH, and then extracted with ether. The free amine is thus obtained (yield = 74%).The malonate monoester (O) (7.5 g), the amine (5A)-1 (4.14 g) in ethanolic solution (30%) and hydroxybenzotriazole (HOBT) (3.97 g) in 70 ml of THF are placed in a 500 ml three-necked flask. After complete dissolution, the whole is cooled to -7C and DCC (5.5 g) diluted in 30 ml of THF is then added dropwise over 30 minutes.The mixture is allowed to warm to room temperature and is then left stirring for 19 hours. At room temperature, the medium becomes cloudy (white precipitate).The precipitate (dicyclohexyl urea) is filtered off and concentrated to dryness. 15.77 g of a beige-coloured solid are obtained.This crude solid is taken up in ethyl acetate (400 ml) and washed with:- HCMN (150 ml)- saturated sodium hydrogen carbonate solution (NaHCO3) (150 ml)- saturated NaCI solution (150 ml) – water (150 ml).After drying over MgSO4 and evaporating off the solvent, 9.34 g of a beige-coloured solid are obtained.YId: 84% m.p. = 1200C 1H NMR (DMSO delta in ppm): 1.08 (s, 3H); 3.41 (t, 2H); 3.93 (t, 2H); 4.07 (q, 2H);6.89 (t, 2H); 7.08 (t, 2H); 7.31 (s, 4H); 7.83 (s, 1H); 8.60 (t, 1H).Purity = 67%MS (APCI) m/z: 419 [M+H]+
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-(4-Fluorophenoxy)ethylamine, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; MERCK PATENT GMBH; WO2008/6432; (2008); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem