4-Iodo-1-Methyl-piperidine synthesis

Yield:363593-53-7 50%

Reaction Conditions:

with 1H-imidazole;iodine;triphenylphosphine in dichloromethane at 0; for 18 h;

Steps:

34.1 Step 1 4-iodo-1-methylpiperidine

4-Hydroxy-1-methylpiperidine 34a (2.3 g, 20 mmol), triphenylphosphine (6.81 g, 26 mmol), imidazole (2.04 g, 30 mmol) and dichloromethane (100 mL) were mixed and cooled down to 0° C., and then added iodine (6.09 g, 24 mmol), and stirring continued for 18 hours, after the reaction was over, it was quenched with water, and then extracted with dichloromethane (50 mL*2), the organic phases were combined and dried over anhydrous sodium sulfate, the desiccant was removed by filtering, and the reaction system was concentrated under reduced pressure, the residue was purified by silica gel column chromatography (dichloromethane/methanol=10/1), so as to obtain the title product 4-iodo-1-methylpiperidine 34b (2.25 g, white solid), and the yield was 50%. MS m/z (ESI): 226[M+H]

References:

US2019/210997,2019,A1 Location in patent:Paragraph 0343; 0344; 0345