ChemicalBook CAS DataBase List CLONIDINE

CLONIDINE synthesis

8synthesis methods

Product Name:CLONIDINE
CAS Number:4205-90-7
Molecular formula:C9H9Cl2N3
Molecular Weight:230.09

21709-18-2 Synthesis

CarboniMidic dichloride, (2,6-dichlorophenyl)-

21709-18-2
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4205-90-7
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Yield:4205-90-7 66 g

Reaction Conditions:

with ethylenediamine in dichloromethane at 5 - 20; for 2 h;

Steps:

3.B B. Synthesis of Intermediate 2
Add 85 ml of thionyl chloride and 110 g of intermediate 1 to the reaction flask, and cool the ice water bath to 0° C. and add 150 ml.A mixture of thionyl chloride and 150 ml of sulfuryl chloride. Naturally warmed to room temperature after joining.After heating to 60 ° C, the reaction was stirred for 22 h, and the system was dissolved and distilled to a fraction without distillation.Add 350 ml of dichloromethane, cool to 5 ° C in an ice water bath, add 130 g of ethylenediamine in dichloromethane, and add dropwise.The temperature was naturally raised to room temperature, and the reaction was stopped for 2 hours. After the reaction was completed, 200 ml of water was added to the system, and the mixture was stirred for 50 minutes.The layers were allowed to stand, the aqueous phase was extracted with dichloromethane (180 ml*2), the aqueous phase was discarded, and the organic phases were combined.Washed 3 times with water, 4 times with 10% sodium hydroxide, and washed 3 times with saturated brine.The dichloromethane layer was collected to give Intermediate 2. Intermediate 2 was added with 300 ml of absolute ethanol, and 767 needles were activated carbon.Stir the mixture to reflux, filter while hot, add 30 mL of hydrogen chloride-ethanol solution, and drop.Stir for 40 min, cool to room temperature, cool to 0 ° C, stir and crystallize for 2.5 h, filter,The filter cake was rinsed with a small amount of ethanol, and dried to obtain clonidine hydrochloride, and clonidine hydrochloride was dissolved in 330 mL of water.Stir at room temperature for 2 h, remove insoluble matter by filtration, and cool to below 10 ° C in an ice water bath.Adjust the pH to 11 with 25% sodium hydroxide to form a white precipitate.Filter, filter cake rinse with a small amount of water,White solid 66g.

References:

Kunming Yuanrui Pharmaceutical Co., Ltd.;Wang Gaohua;Xu Chunxia;Niu Shuwei;Wang Yanchang CN107915679, 2018, A Location in patent:Paragraph 0048; 0055; 0058; 0061; 0062

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