tert-Butyl methyl ether → HCID 66615617, compound

Participants

Reaction Steps

A solution of lithium hydroxide monohydrate (30.5 g) in water (180 mL) was added dropwise to an ice cooled solution of methyl (2S)-2-(4-{[4-(3,4-dichloro-2-methylphenoxy)piperidin-1-yl]methyl}piperidin-1-yl)-3-phenylpropanoate (from step A) in methanol (115 mL) and THF (450 mL). The mixture was stirred at room temperature overnight. A solution of ammonium acetate (165 g) in water (300 mL) was added to the reaction mixture, followed by tert-butylmethyl ether (300 mL). The two phase mixture was stirred rapidly for 2 h. The solid was collected, washed with water (3×300 mL) and diethyl ether (3×200 mL). The solid was added to diethyl ether and stirred for 1 h then filtered. Fresh diethyl ether was added and the stirring, filtering procedure was repeated. The solid obtained was dried under vacuum at 50° C. overnight to give the title compound (33 g).

Provenance & Evidence