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ChemicalBook CAS DataBase List 1-Methylpiperdin-4-ylmagnesium chloride, 0.50 M in THF

1-Methylpiperdin-4-ylmagnesium chloride, 0.50 M in THF synthesis

2synthesis methods
5570-77-4 Synthesis
4-Chloro-N-methylpiperidine

5570-77-4
354 suppliers
$14.00/5g

-

Yield:-

Reaction Conditions:

with magnesium;iodine in tetrahydrofuran for 1 h;Heating / reflux;

Steps:

1
A dried, three-necked flash equipped with argon inlet, a dropping funnel and a thermometer was charged with magnesium turnings (2.52 g, 0.10 mol), which before use had been washed with 0.01 M H2SO4 (aq.) and dried. A small amount of dry THF was added to cover the magnesium. A crystal of iodine was added followed by dibromoethane. When the vigorous reaction had subsided, a solution of distilled 4-chloro-l-methylpiperidine (9.20 g, 0.07 mol) in THF (70 mL) was added dropwise. When the addition was complete, the reaction mixture was heated to refluxing with stirring for 1 h. The reaction mixture was EPO then allowed to cool to room temperature. Full conversion was confirmed by hydrolysis (GC) and generation of Grignard reagent by iodolysis (GC).

References:

ACADIA PHARMACEUTICALS INC. WO2007/47776, 2007, A1 Location in patent:Page/Page column 46; 47