4-[(4-bromophenyl)methyl]piperidine

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1 M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1 M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness

反応条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 4-(4-bromobenzyl)-piperidine (290 mg, 1.14 mmol), formic acid (12 mL) and 37% aqueous formaldehyde (0.30 mL, 3.75 mmol) was divided into three portions. Each portion was heated at 150° C. for 5 minutes in a microwave reactor. The combined cold mixture was loaded onto a 5 g SCX-2 cartridge which was then washed with methanol (30 mL) then 2 N ammonia in methanol (50 mL). Concentration of the combined basic fractions in vacuo gave the title compound (300 mg, 98%) as a colourless oil. LCMS (Method B): RT=2.18 min, M+H+=268, 270. was then washed with methanol (30 mL)

反応条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 4-(4-bromobenzyl)-piperidine (290 mg, 1.14 mmol), formic acid (12 mL) and 37% aqueous formaldehyde (0.30 mL, 3.75 mmol) was divided into three portions. Each portion was heated at 150° C. for 5 minutes in a microwave reactor. The combined cold mixture was loaded onto a 5 g SCX-2 cartridge which was then washed with methanol (30 mL) then 2 N ammonia in methanol (50 mL). Concentration of the combined basic fractions in vacuo gave the title compound (300 mg, 98%) as a colourless oil. LCMS (Method B): RT=2.18 min, M+H+=268, 270. was then washed with methanol (30 mL)

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1 M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1 M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness

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

実験手順: To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%). The solvent was removed in vacuo the residue dissolved into CH2Cl2 (50 mL) washed with NaOH (0.1M, 10 mL), brine (10 mL) dried over MgSO4 concentrated to dryness