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CAS No. : | 109-07-9 | MDL No. : | MFCD00005954 |
Formula : | C5H12N2 | Boiling Point : | - |
Linear Structure Formula : | (CH3)C4H9N2 | InChI Key : | JOMNTHCQHJPVAZ-UHFFFAOYSA-N |
M.W : | 100.16 | Pubchem ID : | 66057 |
Synonyms : |
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Signal Word: | Danger | Class: | 4.1 |
Precautionary Statements: | P210-P240-P241-P261-P264-P271-P280-P302+P352-P304+P340+P312-P305+P351+P338-P332+P313-P337+P313-P370+P378-P403+P233-P405-P501 | UN#: | 1325 |
Hazard Statements: | H228-H315-H319-H335 | Packing Group: | Ⅱ |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | In butan-1-ol; at 120℃; for 0.333333h; | a) Synthesis of 2-(3-methylpiperazine-1-yl)-1,3,4-thiadiazol 2.0 g (12.1 mmol) 2-bromine-[1,3,4]-thiadiazol and 7.2 g (72.7 mmol) 2-methylpiperazine were stirred in n-butanol (10 ml) for 20 min at 120 C. The mixture was subsequently concentrated in a vacuum. CC (SiO2, DCE/EtOH/conc. NH4OH 5:1:0.06) was performed with the residue, whereby 1.7 g (9.3 mmol, 78%) 2-(3-methylpiperazine-1-yl)-1,3,4-thiadiazol was obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48 g | In isopropyl alcohol;Reflux; | (Comparative Example 2) (±) -2- methylpiperazine 15.0g (0.15mol), (R) -2- phenoxypropionicacid 69.8 g (0.42 mol), was mixed 2-propanol 250 ml, heated to reflux the contents, lysis did.After dissolution, the solution was cooled overnight to 25 C. The resulting separated crystalswere dried to give crude diastereomeric salt 48.0 g. [Α] D: + 21.2 (C = 1.0, methanol). (In FIG. 2, 2 crystallization, 3 crystallization was described as) The crude diastereomeric salt of 2-propanol from twice recrystallized by, purified diastereomeric salt (R)-2-methylpiperazine three ((R) -2-phenoxypropionic acid) 41.3g. [Α] D: + 23.0 (C = 1.0, methanol) melting point 149 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80.67% | Put 3.3 g of boric acid, 17.8 ml of acetic anhydride, and 0.1 g of zinc chloride in the reaction bottle.After fully mixed, it is heated to 110 C and cooled to 60 C after 1 hour.11.5 g of ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxoquinolinyl 3-carboxylate obtained above was added and heated To 80 , cool after 2h,After washing with water, perform suction filtration treatment, and then wash with distilled water 3 times,After drying, 12.73 g of a pale yellow solid was obtained with a yield of 90.43%.Add 24 ml of acetonitrile, 8 ml of triethylamine, and10g compound 1-cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxoquinolinyl-3-carboxylic acid diacetate boron chelate and 2.6g of 2-methylpiperazine,Stir at room temperature for more than 10 hours. After concentration and filtration, wash with water.120 ml of 95% ethanol and 24 ml of triethylamine were added, and the mixture was heated under reflux for 6 hours and then cooled. After filtration, the filtrate was concentrated.Finally, 100 ml of ethanol was added to dissolve the concentrated preparation of the above filtrate,Then adjust the pH to 7.0 with dilute hydrochloric acid, and vacuum dry to obtain 8.2g white solid,That is gatifloxacin, the yield is 80.67%, and the overall yield is 41.45%. |