4-(3,5-DICHLOROPHENOXY)PIPERIDINE synthesis

Yield:254883-39-1 71%

Reaction Conditions:

Stage #1: tert-butyl 4-(3,5-dichlorophenoxy)piperidine-1-carboxylatewith hydrogenchloride in 1,4-dioxane at 20 - 50; for 12.1667 h;
Stage #2: with sodium hydroxide in dichloromethane;water;

Steps:

1.2

To a solution of 3 (2.10 g, 6.07 mmol) in 1 ,4-dioxane (15 ml) was added HCI (4.0 M in 1 ,4-dioxane, 15.0 ml, 60.0 mmol) at RT. The reaction mixture was heated at 50⁰C for 10 min., and then stirred at RT for 12 h. The solvent was removed by reduced pressure, followed by addition of CH₂CI₂ and 1.0 M aqueous NaOH solution. The organic layer was separated, dried over MgSO₄, and concentrated in vacuo. 1.06 g of crude residue 4 (71%) was obtained as a colorless oil and used in the next reaction without further purification.

References:

WO2007/1975,2007,A1 Location in patent:Page/Page column 25