1-[2-(2-Hydroxyethoxy)Ethyl]Piperidine synthesis

Yield:3603-43-8 42%

Reaction Conditions:

with potassium carbonate in 1,4-dioxane at 70;

Steps:

13.1

Compound 1-3 (2.6 g, 10 mmol) was dissolved in 1,4-dioxane (40 mL), followed by addition of piperidine 13-1 (2.52 g, 30 mmol), and potassium carbonate (2.76 g, 20 mmol) was added under stirring, followed by stirring the reaction overnight under conditions of 70° C. and a closed reaction system, TLC monitoring showed that the starting material 1-3 was completely reacted. The solvent was removed under reduced pressure to obtain a concentrated residue. The concentrated residue was dispensed with dichloromethane (20 mL), an appropriate amount of silica gel was added and the sample was stirred, spin-dried under reduced pressure and directly placed on a silica gel column for column chromatographic purification, with an eluent (dichloromethane:methanol=20/1-5/1) to obtain the target product 13-2 (0.73 g, 42%) as a pale yellow oil, LC-MS: m/z=174[M+H]⁺.

References:

US2017/2028,2017,A1 Location in patent:Paragraph 0129; 0130