4-(2-chloro-4-fluorophenoxy)piperidine

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: DEAD (0.90 ml) was added to a solution of triphenylphosphine (1.44 g), 2-chloro-4-fluorophenol (0.806 g) and 4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (1.0 g) in THF at RT. The reaction was stirred for 16 hrs, HCl (2 ml, 4M in dioxan) added and the mixture stirred at RT for 16 hrs. The mixture was then evaporated to dryness, triethylamine (5 ml) added, re-evaporated, dissolved in methanol (10 ml) and placed on to a SCX cartridge (Varian, 10 g), eluted first with methanol then with 10% NH3 in methanol. The basic fractions were combined and evaporated to give the sub-title compound as an oil (0.98 g) the mixture stirred at RT for 16 hrs The mixture was then evaporated to dryness, triethylamine (5 ml) added re-evaporated dissolved in methanol (10 ml) eluted first with methanol evaporated

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: DEAD (0.90 ml) was added to a solution of triphenylphosphine (1.44 g), 2-chloro-4-fluorophenol (0.806 g) and 4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (1.0 g) in THF at RT. The reaction was stirred for 16 hrs, HCl (2 ml, 4M in dioxan) added and the mixture stirred at RT for 16 hrs. The mixture was then evaporated to dryness, triethylamine (5 ml) added, re-evaporated, dissolved in methanol (10 ml) and placed on to a SCX cartridge (Varian, 10 g), eluted first with methanol then with 10% NH3 in methanol. The basic fractions were combined and evaporated to give the sub-title compound as an oil (0.98 g) the mixture stirred at RT for 16 hrs The mixture was then evaporated to dryness, triethylamine (5 ml) added re-evaporated dissolved in methanol (10 ml) eluted first with methanol evaporated