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ChemicalBook CAS DataBase List Tizanidine

Tizanidine synthesis

4synthesis methods
30536-19-7 Synthesis
4-Amino-5-chloro-2,1,3-benzothiadiazole

30536-19-7
241 suppliers
$27.00/5g

1H-Imidazole, 2-chloro-4,5-dihydro-, hydrochloride (1:1)

54255-14-0
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Yield:51322-75-9 90.5%

Reaction Conditions:

with pyridine in iso-butanol at 65 - 70; for 8 h;Temperature;Solvent;Reagent/catalyst;

Steps:

10
Weigh 50g 4-amino-5-chloro-2,1,3-benzothiadiazole, 76g 2-chloro-2-imidazoline hydrochloride,85.2 g of pyridine, added to 1000 mL of sec-butanol,Raise to 65-70 ° C and stir for 8 hours.TLC detected the end of the reaction. Pour the reaction solution intoIn 2000 mL of ice water, the control temperature does not exceed 20 °C.Add 20% sodium hydroxide to adjust the pH to 9-10.The control temperature is not higher than 30 °C. filter,The filter cake was recrystallized from methanol. Detizeidine 61.8g,The yield was 90.5%, and the HPLC purity was 99.18%.

References:

Sichuan Keruide Pharmaceutical Co., Ltd.;Liu Qiangwei;Li Xiaoli;Fu Lin;Chen Gang CN109535148, 2019, A Location in patent:Paragraph 0012; 0042-0043; 0045-0046; 0048-0049; 0051-0052

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