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[ CAS No. 17512-61-7 ] {[proInfo.proName]}

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Chemical Structure| 17512-61-7
Chemical Structure| 17512-61-7
Structure of 17512-61-7 * Storage: {[proInfo.prStorage]}
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Product Details of [ 17512-61-7 ]

CAS No. :17512-61-7 MDL No. :MFCD07787461
Formula : C9H6BrClS Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 261.57 Pubchem ID :-
Synonyms :

Safety of [ 17512-61-7 ]

Signal Word:Danger Class:8
Precautionary Statements:P264-P270-P271-P280-P303+P361+P353-P304+P340-P305+P351+P338-P310-P330-P331-P363-P403+P233-P501 UN#:3261
Hazard Statements:H302-H314 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 17512-61-7 ]

* 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.

  • Downstream synthetic route of [ 17512-61-7 ]

[ 17512-61-7 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 17512-61-7 ]
  • [ 24155-42-8 ]
  • [ 99592-32-2 ]
YieldReaction ConditionsOperation in experiment
With sodium hydroxide;tetra(n-butyl)ammonium hydrogensulfate; In toluene; at 35 - 40℃; for 3.25h; Example 1: Sertaconazole mononitrate monohydrate (V) (Sertaconazole mononitrate pseudopolymorph)A 2-L flask was loaded with 308 mL of toluene, 100 g of 1- (2,4-dichlorophenyl) -2- (lH-imidazol-1-yl) -ethanol (II) (0.389 mol) and 6.67 g of tetrabutylammonium hydrogen sulfate (IV, Z = HSO4) (0.0196 mol) . Then, 155 g of sodium hydroxide (purity 49%; 1.905 mol) were added. The mixture was heated at 35-4O0C and stirred for 15 minutes. A solution comprising 111.11 g of 3-bromomethyl-7- chlorobenzo [Jb] thiophene (III) (0.425 mol) and 595 mL of toluene, maintaining the mass temperature between 37 and 400C, was added for at least 30 minutes. After the addition, the system was maintained between 37 and 400C for 2.5 hours and thereafter water (635 mL ) was added. The mixture was cooled to a mass temperature of 5-100C and the sertaconazole precipitated was filtered and washed with water and cold toluene (5-1O0C), obtaining 179.7 g of wet sertaconazole free base(161.7 g dry) . The sertaconazole free base obtained was loaded into a 2 L reactor containing 848 mL of absolute ethanol. The mixture was refluxed until complete dissolution. Then the mixture was heated at a mass temperature between 68 and 72C, and 236 mL of water were added. The mixture was cooled at 100C and this temperature was maintained for 1 hour. The solid material formed was filtered and washed with a solution of 160 mL of absolute ethanol and 51 mL of water previously- cooled at 100C. Wet pure sertaconazole free base (177.9 g) was obtained (158 g dry) . The obtained pure sertaconazole free base was loaded into a 2 L reactor and re-dissolved with 932 mL of absolute ethanol at 750C. The mixture was then cooled at a mass temperature of 67-700C and a solution containing 53.7 g (0.512 mol) of 60% nitric acid in 193 mL of water is added. The temperature was stabilized for 15 minutes, checking that the pH was maintained below 2. The mixture was cooled at 100C and kept for 1 hour. The precipitated material was filtered and washed with water, providing 215.9 g of sertaconazole mononitrate monohydrate (V) (Sertaconazole mononitrate pseudopolymorph) . Yield 88.7%.Analytical dataIR (infrared) : A Magna-IR 550 Nicolet spectrometer with a database running in Omnic 2.1 software has been used. The recorded IR spectrum of sertaconazole mononitrate monohydrate (V) compared to sertaconazole mononitrate (I) is shown in Figure 2/5.DSC (differential scanning calorimetry) : A Mettler' TA-8000 instrument comprising DSC-820 and TG-50 components, and a MT-5 balance provided with a database running in TAS 810 1.1 software has been used. A product sample of 1 to 5 mg was weighted in a 40 muL aluminum crucible, maintaining the following conditions: Temperature range: 110-1800C Heating speed: 100C / min Nitrogen flow: 100 mL / min The recorded DSC of sertaconazole mononitrate monohydrate (V) compared to sertaconazole mononitrate (I) is shown in Figure 3/5.Microscopy: A Nikon-Eclipse E-600 unit with polarized light, provided with a Linkam THMS 600 heating plate and a Linksys database and image manager software has been used. Some product particles were suspended in mineral oil on a glass slide and the sample was examined by magnification depending on the particle size and using polarized light or not . Sertaconazole mononitrate monohydrate (V) and sertaconazole mononitrate (I) microphotographs are shown in Figure 4/5.X Rays Diffraction: A Siemens powder X Ray Diffraction Equipment model D-500 has been used. The X Rays diffractograms for sertaconazole mononitrate monohydrate (V) and sertaconazole mononitrate (I) are shown in Figure 5/5. The crystal data and structure refinement for sertaconazole mononitrate monohydrate (V) are shown in Table 2. Table2Crystal data and structure refinement for sertaconazole mononitrate monohydrate (V) Empirical formula C20H15CI3N2OS. HNO3. H2O Formula weight 518.78 Temperature 293(2)K Wavelength 0.71069 A Crystal system Monoclinic Space group P2i/c a = 16.049(2)A alpha = 90 Unit cell dimensions b = 8.946(7)A beta = 102.046(7) c = 15.990(3) A Y = 90 Volume 2245(2) A3 Z 4 Density (calculated) 1.535 Mg/m3 Absorption coefficient 0.540 mm"1 Crystal size 0.1 x 0.1 x 0.2 mm Theta range for data collection 1.30 to 30.07 Index ranges -3<h<16, -12<k<12, -22<l<21 Reflections collected 11440 Independent reflections 5861 [R(int) = 0.1748] Refinement method Full-matrix least-squares on F2 Data / restraints / parameters 3246 / 1 /336 Goodness-of-fit on F2 0.980 Final R indices [l>2?(l)] R1 = 0.0644, WR2 = 0.1302 R indices (all data) R1 = 0.3270, WR2 = 0.2365 Extinction coefficient 0.0000(6) Largest diff. peak and hole 0.356 and -0.429 e.A3
  • 2
  • [ 17512-61-7 ]
  • [ 24155-42-8 ]
  • [ 99592-39-9 ]
YieldReaction ConditionsOperation in experiment
95.7% Stage #1: 3-Bromomethyl-7-chlorobenzo<b>thiophene; 1-(2,4-dichlorophenyl)-2-(1H-imidazol-1-yl)ethan-1-ol With tetrabutyl-ammonium chloride; sodium hydroxide In water; toluene at 80℃; for 4h; Stage #2: With nitric acid 1.4; 2-4; 1-4 (4) Salt formation Add 16.58kg of water, 2.98kg of sodium hydroxide, and 43.28kg of toluene into the reaction kettle; Then add 3.36kg of 50% tetrabutylammonium chloride aqueous solution, 3-bromomethyl-7-chlorobenzo[b]thiophene 12.96kg, 10.76 kg of 1-(2,4-dichlorophenyl)-2-(1-imidazol-1-yl)ethanol was heated to 80°C and stirred at constant temperature for 4 hours. Cool, stand for layering, collect the toluene layer, add 36.42 kg of ether and 98.76 kg of water, stir, place until the precipitation is complete, and filter. The filtrate is pumped back to the reaction kettle for layering. Concentrated nitric acid 3.50kg was added dropwise to the organic layer to precipitate solids, which were filtered and washed with water, and washed with ether. 23.04 kg of crude sertaconazole nitrate was obtained with a purity of 90.04%. Example 2-Purification of Sertaconazole Nitrate The crude sertaconazole nitrate of Example 1 was refined with 3.0 kg, and the specific operations were as follows: Add 20kg of 95% ethanol into the reaction kettle, start stirring, and at the same time turn on steam heating, raise the temperature to 60°C, add 3.0kg crude sertaconazole nitrate while stirring, and reflux for 1 hour. Adding 90g of activated carbon, the activated carbon is prepared by mixing coconut shell activated carbon, litchi husk activated carbon and copper-zinc modified activated carbon at a mass ratio of 1:1.3:0.4. The pore diameters of the three are 1000-1100nm, respectively. 400-500nm, 700-800nm; Incubate at 60 °C - 65 °C for 15 minutes, filter while hot. The filtrate is filtered into a refining kettle, the temperature is lowered, and crystals are precipitated out of standing. The crystalline liquid was filtered and the crystals were taken out. Pour the crystals into a centrifuge to filter, take the material, place it in a clean and dry baking tray, mash the filter cake with a stainless steel spatula, and flatten it. Put it into a vacuum drying oven to dry, and get the finished product of sertaconazole nitrate. Inner packaging, outer packaging, and storage.
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