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ChemicalBook CAS DataBase List pridinol
511-45-5

pridinol synthesis

4synthesis methods
-

Yield:511-45-5 79.69%

Reaction Conditions:

Stage #1:methyl 3-(piperidino)propionate;phenylmagnesium bromide in tetrahydrofuran at 0 - 66; for 3 h;
Stage #2: with hydrogenchloride;water in tetrahydrofuran at 0;

Steps:

2 Example 2
An example was added to a three-necked flask equipped with a mechanical stirrer and drying tube1 to a solution of methyl 3- (1-piperidinyl) propionate(85.70 g, 0.50 mol) was added300 mL of tetrahydrofuran0 ° C,Began to drop the phenyl magnesium bromide Grignard reagent,Drop finished,Heating up to 66 ,The reaction was stirred for 3 h.The reaction system was then cooled to 0 ° C,A solution of 1 L of 4 M HCl was added dropwise.Hydrolysis is completed,Dispensing,The aqueous phase was extracted with 3 x 400 ml of chloroform,Combine organic phase,Organic phase used500 ml of saturated sodium chloride solution,Dispensing,The organic phase was dried over anhydrous sodium sulfate.The tetrahydrofuran and chloroform were removed by steaming,After drying,To obtain a light yellow solid(123.73 g, yield 83.77%).123.73 g was added to 500 ml of ethanol to recrystallize,It was possible to obtain a pale yellow needle-like crystals of Prudential (117.71 g, yield 79.69%).

References:

Hubei University of Technology;Wang, Wei;Zhou, Baohan;Sun, Dan;Hu, Lixin;Li, Linglan;Miao, Junfeng;Ren, Jiaqiang CN104262290, 2017, B Location in patent:Paragraph 0018; 0019; 0020

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