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[ CAS No. 51322-75-9 ] {[proInfo.proName]}

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Chemical Structure| 51322-75-9
Chemical Structure| 51322-75-9
Structure of 51322-75-9 * Storage: {[proInfo.prStorage]}
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Product Details of [ 51322-75-9 ]

CAS No. :51322-75-9 MDL No. :MFCD00865192
Formula : C9H8ClN5S Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 253.71 Pubchem ID :-
Synonyms :

Safety of [ 51322-75-9 ]

Signal Word:Warning Class:
Precautionary Statements:P201-P202-P264-P270-P280-P301+P312+P330-P308+P313-P220-P405-P501 UN#:
Hazard Statements:H302-H361 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 51322-75-9 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Upstream synthesis route of [ 51322-75-9 ]
  • Downstream synthetic route of [ 51322-75-9 ]

[ 51322-75-9 ] Synthesis Path-Upstream   1~1

  • 1
  • [ 51322-75-9 ]
  • [ 64461-82-1 ]
YieldReaction ConditionsOperation in experiment
83.5% With hydrogenchloride In ethanol at 20℃; for 2 h; 18.6 g of 4-amino-5-chloro-2,1,3-benzothiadiazole and 15.4 g of 1-acetylimidazolin-2-one were weighed and added to 120 ml of phosphorus oxychloride to raise the temperature to 60 to 65. °C reaction for 36 hours. The solvent was evaporated under reduced pressure, 160 ml of methanol was added to the obtained oil, and the mixture was heated to reflux for 4 hours. After cooling to room temperature, the reaction solution was poured into 160 ml of ice water, and the pH of the aqueous solution of sodium hydroxide was adjusted to 9-10. Filter and dry. 17.8 g of powdered solid tizanidine was obtained in a yield of 70percent.The resulting tizanidine was added to 100 ml of a saturated ethanolic hydrogen chloride solution and stirred at room temperature for 2 hours. After filtration, the filter cake was washed with anhydrous ethanol and dried. The filter cake was added to 200 ml of 95percent ethanol, refluxed until completely dissolved, naturally cooled, crystallized, filtered, and the filter cake was washed with anhydrous ethanol and dried to obtain solid tizanidine hydrochloride 17 g in a yield of 83.5percent with a purity of 99.22percent.
37.9 g
Stage #1: With acetic acid In acetone for 2 h; Reflux
Stage #2: With hydrogenchloride In water; acetone for 2 h; Reflux
Tizanidine 45g was added to 180mL of acetone,Heated to reflux,21.3 g of acetic acid was added,Solution clarification,Slow down to a solid precipitation,Keep heating for 2 hours,And then cool down to 0 ° C below,Crystallization for 3 hours,filter,Dried to give 51.4 g of crude tizanidine acetate as an off-white solid, the yield was 92.4percentDirectly for the next step. Tizanidine acetate crude 50g,Was added to 200 mL of acetone,Heated to reflux,24 g of acetic acid was added,Solution clarification,10 mL of hydrochloric acid was added,Slow down to a solid precipitation,Insulation reaction 2 hours,And then cool to 0-10 ° C,Crystallization for 3 hours,filter,Dried to give 39.7 g of tizanidine hydrochloride as a white solid,The yield was 87.8percentPurity of 99.9percent.
Reference: [1] Patent: CN107778307, 2018, A, . Location in patent: Paragraph 0044-0046; 0047-0048; 0049-0050
[2] Patent: CN106946874, 2017, A, . Location in patent: Paragraph 0038-0040; 0041-0043; 0044-0046
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