N-(2-phenylethyl)benzamide

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: To a solution of benzoyl chloride (0.123 moles) (Aldrich) in 600 mL of CH2Cl2 was added 2.0 eq. of phenethylamine (Aldrich) dropwise. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separatory and extracted with CH2Cl2. The organic extracts were washed with water and 1N HCl, and then dried over Na2SO4, filtered and concentrated to give N-phenethyl benzamide. poured into a separatory and extracted with CH2Cl2 The organic extracts were washed with water and 1N HCl dried over Na2SO4 filtered concentrated

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

実験手順: To a solution of benzoyl chloride (0.123 moles) (Aldrich) in 600 mL of CH2Cl2 was added 2.0 eq. of phenethylamine (Aldrich) dropwise. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separatory and extracted with CH2Cl2. The organic extracts were washed with water and 1N HCl, and then dried over Na2SO4, filtered and concentrated to give N-phenethyl benzamide. poured into a separatory and extracted with CH2Cl2 The organic extracts were washed with water and 1N HCl dried over Na2SO4 filtered concentrated

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

実験手順: To a solution of benzoyl chloride (0.123 moles) (Aldrich) in 600 mL of CH2Cl2 was added 2.0 eq. of phenethylamine (Aldrich) dropwise. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separatory and extracted with CH2Cl2. The organic extracts were washed with water and 1N HCl, and then dried over Na2SO4, filtered and concentrated to give N-phenethyl benzamide. poured into a separatory and extracted with CH2Cl2 The organic extracts were washed with water and 1N HCl dried over Na2SO4 filtered concentrated

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

実験手順: 17.6 Grams of a 50% solution of n-propane-phosphonic acid anhydride in methylene chloride are added in 3 portions, with stirring and the exclusion of moisture, to a solution of 2.4 g of β-phenylethylamine, 2.2 g of benzoic acid and 14 ml of N-ethyl morpholine in 25 ml of methylene chloride. The temperature rises to about +40° C. The mixture is cooled to room temperature, while stirring, and is worked up after 24 hours of standing by adding 350 ml of methylene chloride and extracting the solution three times with 50 ml each of water, saturated sodium carbonate solution and potassium bisulfate solution. The crude product crystallizes from the methylene chloride solution dried over magnesium sulfate. Said product is filtered off with suction together with a small amount of petroleum ether (boiling point 40° to 60° C.). rises to about +40° C while stirring extracting the solution three times with 50 ml each of water, saturated sodium carbonate solution and potassium bisulfate solution The crude product crystallizes from the methylene chloride solution dried over magnesium sulfate is filtered off with suction together with a small amount of petroleum ether (boiling point 40° to 60° C.)

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

実験手順: 17.6 Grams of a 50% solution of n-propane-phosphonic acid anhydride in methylene chloride are added in 3 portions, with stirring and the exclusion of moisture, to a solution of 2.4 g of β-phenylethylamine, 2.2 g of benzoic acid and 14 ml of N-ethyl morpholine in 25 ml of methylene chloride. The temperature rises to about +40° C. The mixture is cooled to room temperature, while stirring, and is worked up after 24 hours of standing by adding 350 ml of methylene chloride and extracting the solution three times with 50 ml each of water, saturated sodium carbonate solution and potassium bisulfate solution. The crude product crystallizes from the methylene chloride solution dried over magnesium sulfate. Said product is filtered off with suction together with a small amount of petroleum ether (boiling point 40° to 60° C.). rises to about +40° C while stirring extracting the solution three times with 50 ml each of water, saturated sodium carbonate solution and potassium bisulfate solution The crude product crystallizes from the methylene chloride solution dried over magnesium sulfate is filtered off with suction together with a small amount of petroleum ether (boiling point 40° to 60° C.)

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

実験手順: To a solution of benzoyl chloride (0.123 moles) (Aldrich) in 600 mL of CH2Cl2 was added 2.0 eq. of phenethylamine (Aldrich) dropwise. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separatory and extracted with CH2Cl2. The organic extracts were washed with water and 1N HCl, and then dried over Na2SO4, filtered and concentrated to give N-phenethyl benzamide. poured into a separatory and extracted with CH2Cl2 The organic extracts were washed with water and 1N HCl dried over Na2SO4 filtered concentrated

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

実験手順: To a solution of benzoyl chloride (0.123 moles) (Aldrich) in 600 mL of CH2Cl2 was added 2.0 eq. of phenethylamine (Aldrich) dropwise. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separatory and extracted with CH2Cl2. The organic extracts were washed with water and 1N HCl, and then dried over Na2SO4, filtered and concentrated to give N-phenethyl benzamide. poured into a separatory and extracted with CH2Cl2 The organic extracts were washed with water and 1N HCl dried over Na2SO4 filtered concentrated

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

実験手順: To a solution of benzoyl chloride (0.123 moles) (Aldrich) in 600 mL of CH2Cl2 was added 2.0 eq. of phenethylamine (Aldrich) dropwise. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separators and extracted with CH2Cl2. The organic extracts were washed with water and 1N HCl, and then dried over Na2SO4, filtered and concentrated to give N-phenethyl benzamide. poured into a separators extracted with CH2Cl2 The organic extracts were washed with water and 1N HCl dried over Na2SO4 filtered concentrated

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

実験手順: To a solution of benzoyl chloride (0.123 moles) (Aldrich) in 600 mL of CH2Cl2 was added 2.0 eq. of phenethylamine (Aldrich) dropwise. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separatory and extracted with CH2Cl2. The organic extracts were washed with water and 1N HCl, and then dried over Na2SO4, filtered and concentrated to give N-phenethyl benzamide. poured into a separatory and extracted with CH2Cl2 The organic extracts were washed with water and 1N HCl dried over Na2SO4 filtered concentrated

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

実験手順: To a solution of benzoyl chloride (0.123 moles) (Aldrich) in 600 mL of CH2Cl2 was added 2.0 eq. of phenethylamine (Aldrich) dropwise. The reaction mixture was stirred at room temperature for 3 hours and then poured into a separatory and extracted with CH2Cl2. The organic extracts were washed with water and 1N HCl, and then dried over Na2SO4, filtered and concentrated to give N-phenethyl benzamide. poured into a separatory and extracted with CH2Cl2 The organic extracts were washed with water and 1N HCl dried over Na2SO4 filtered concentrated

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

実験手順: 75.5 g (532 mmol, 1.2 eq.) of P2O5 are added with stirring to a solution of 100.0 g (446 mmol) of N-(2-phenylethyl)benzamide in 375 ml of xylene. 124.1 ml (1.34 mol, 3.0 eq.) of PPCl3 are subsequently added, and the reaction mixture is refluxed with TLC monitoring. When the conversion is complete, the reaction solution is poured while hot onto ice and carefully adjusted to pH=12 using 20% NaOH. The phosphate which precipitates in the process is dissolved by addition of water. The product is subsequently extracted with toluene, converted into the hydrochloride using 1 N HCl and extracted with sufficient water. The aqueous phase is rendered basic again using 20% NaOH with ice-cooling, the reaction product is extracted with toluene, dried over MgSO4 and evaporated to dryness under reduced pressure, giving 89.7 g (432.9 mmol) of a viscous yellow oil, corresponding to 97% of theory. the reaction mixture is refluxed with TLC monitoring the reaction solution is poured while hot onto ice The phosphate which precipitates in the process is dissolved by addition of water The product is subsequently extracted with toluene extracted with sufficient water cooling the reaction product is extracted with toluene dried over MgSO4 evaporated to dryness under reduced pressure