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(S)-1-(3-ethoxy-4-methoxyphenyl)-2-methylsulfonylethylamine L-pyroglutamic acid salt[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
29.7 g
In ethanol; for 0.5h;Reflux;
A stirred solution l-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethanamine (50gm) in 1500ml ethanol was added L-pyroglutamic acid(23.62g) at 25-30C. Then reaction mixture was heated to reflux temperature and stirred for 30 min. Slowly cool the reaction mass to room temperature. Stirred for 12 hr at ambient temperature. The slurry was filtered and wet cake was washed with ethanol. Dry the wet cake under vacuum at 50- 55C for 4.0hr. The crude solid (35g) and ethanol (1155ml) were heated to reflux for 30min, slowly cool the reaction mass to room temperature and stirred for additional 12.0hr at ambient temperature.The slurry was filtered and wet cake was washed with ethanol. The wet cake was dried under vacuum at 50-55C yielding 29.7g of L- Pyroglutamic acid salt of (S)-2-(3-ethoxy-4-methoxyphenyl)-l-(methylsulfonyl) ethanamine. Chiral purity: 99.9%.Chemical Purity: 99.5% IH NMR delta DMSO 1.32, 1.93- 2.29, 2.88, 3.36-3.52, 3.71, 3.96-4.01, 4.335.52 ,6.89, 7.05, 7.79
(S)-1-(3-ethoxy-4-methoxyphenyl)-2-methylsulfonylethylamine L-pyroglutamic acid salt[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In methanol; acetone; at 62℃; for 1h;
Acetone (300 mL), Methanol (42 mL), racemic Amine (100 g) and L-Pyroglutamic acid (21.51 g) were mixed in to the reaction vessel and heated the reaction mass for 1.0 hr. at 62 ± 3C. The reaction mass was cooled to room temperature and filtered the solid. The obtained salt was recrystallised in Acetone (240 mL) and Methanol (18 mL) mixture to get desired purity.
General procedure: To a round bottom flask with a stirring bar, L-pyroglutamic acid(10 mmol), phenol/aromatic amine (11 mmol) and DMAP (1 mmol) in dry CH2Cl2 (30 mL) was stirred for 10 min, followed by addition of DCC(11 mmol). The mixture was allowed to stir at room temperature overnight. The reaction was filtered through a coarse frit and the filtrate diluted with CH2Cl2 (50 mL), washed with brine (3×20 mL), dried over MgSO4, and concentrated to dryness. The crude mixture was purified using flash column chromatography (MeOH/ CH2Cl2=1/30) to give the pure products.
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