1-phenylpropan-2-amine

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Amphetamine-ATP (0.095 g, 3×10-4 mol, Example 12) was dissolved in 50 ml of 0.12M potassium carbonate in 80% methanol/20% water. After 5 min at room temperature the thiol concentration was determined by reaction with DTNB to be 25 mM. The amphetamine thiol (7.6 ml, 1.9×10-4 mol) was added with stirring to 20.3 ml (0.4 g, 5.9×10-6 mol) of SMCC-BSA, 10/1. The pH of the solution was adjusted to 7 with 1N hydrochloric acid. The container was purged with argon and the solution was stirred at room temperature for 2 hr. The conjugate solution was then dialyzed with a PYROSTART ultrafiltration module against 10 mM morpholineethanesulfonic acid, pH 5.77 and 110 ml of 3.57 mg/ml BSA-amphetamine was collected. The protein solution was frozen at -70° C. After 5 min at room temperature the thiol concentration was determined by reaction with DTNB The container was purged with argon The conjugate solution was then dialyzed with a PYROSTART ultrafiltration module against 10 mM morpholineethanesulfonic acid, pH 5.77 and 110 ml of 3.57 mg/ml BSA-amphetamine was collected The protein solution was frozen at -70° C.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Amphetamine-ATP (0.095 g, 3×10-4 mol, Example 12) was dissolved in 50 ml of 0.12M potassium carbonate in 80% methanol/20% water. After 5 min at room temperature the thiol concentration was determined by reaction with DTNB to be 25 mM. The amphetamine thiol (7.6 ml, 1.9×10-4 mol) was added with stirring to 20.3 ml (0.4 g, 5.9×10-6 mol) of SMCC-BSA, 10/1. The pH of the solution was adjusted to 7 with 1N hydrochloric acid. The container was purged with argon and the solution was stirred at room temperature for 2 hr. The conjugate solution was then dialyzed with a PYROSTART ultrafiltration module against 10 mM morpholineethanesulfonic acid, pH 5.77 and 110 ml of 3.57 mg/ml BSA-amphetamine was collected. The protein solution was frozen at -70° C. After 5 min at room temperature the thiol concentration was determined by reaction with DTNB The container was purged with argon The conjugate solution was then dialyzed with a PYROSTART ultrafiltration module against 10 mM morpholineethanesulfonic acid, pH 5.77 and 110 ml of 3.57 mg/ml BSA-amphetamine was collected The protein solution was frozen at -70° C.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The polarization value for a sample is compared to a standard curve prepared using calibrators of known amphetamine or d-methamphetamine content. prepared

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The polarization value for a sample is compared to a standard curve prepared using calibrators of known amphetamine or d-methamphetamine content. prepared

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 7.56 g (50 mmol) of 3-nitrobenzaldehyde, 11.25 g (150 mmol) of nitroethane and 4.24 g (55 mmol) of ammonium acetate was heated in 2 mL of acetic acid in a 110° C. oil bath for 2 1/2 hours. Subsequent examination of the mixture by preparative thin layer chromatography with hexane/ethyl acetate showed almost no starting material remaining. Volatile materials were removed with a rotary evaporator, and the residue was partitioned between dichloromethane and water, with washing of the organic layer twice with 10% sodium bicarbonate. Caution was necessary because gas evolution occurred during the first bicarbonate wash. Drying was performed with magnesium sulfate. Filtration and removal of solvent left 9.13 g of crude product. Half of this was chromatographed on a 3×35 cm flash silica column, packed with hexane and eluted with 7:1 hexane/ethyl acetate to give 1.66 g (32%) of pure title compound. Volatile materials were removed with a rotary evaporator the residue was partitioned between dichloromethane and water with washing of the organic layer twice with 10% sodium bicarbonate wash Drying Filtration and removal of solvent left 9.13 g of crude product Half of this was chromatographed on a 3×35 cm flash silica column eluted with 7:1 hexane/ethyl acetate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 7.56 g (50 mmol) of 3-nitrobenzaldehyde, 11.25 g (150 mmol) of nitroethane and 4.24 g (55 mmol) of ammonium acetate was heated in 2 mL of acetic acid in a 110° C. oil bath for 2 1/2 hours. Subsequent examination of the mixture by preparative thin layer chromatography with hexane/ethyl acetate showed almost no starting material remaining. Volatile materials were removed with a rotary evaporator, and the residue was partitioned between dichloromethane and water, with washing of the organic layer twice with 10% sodium bicarbonate. Caution was necessary because gas evolution occurred during the first bicarbonate wash. Drying was performed with magnesium sulfate. Filtration and removal of solvent left 9.13 g of crude product. Half of this was chromatographed on a 3×35 cm flash silica column, packed with hexane and eluted with 7:1 hexane/ethyl acetate to give 1.66 g (32%) of pure title compound. Volatile materials were removed with a rotary evaporator the residue was partitioned between dichloromethane and water with washing of the organic layer twice with 10% sodium bicarbonate wash Drying Filtration and removal of solvent left 9.13 g of crude product Half of this was chromatographed on a 3×35 cm flash silica column eluted with 7:1 hexane/ethyl acetate