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Practical pharmaceutical chemistery

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Marwa Abd El Kader
Marwa Abd El Kader

Identification & Assay of Aspirin ,Isonicotinic acid Hydrazide (I.N.H) ,Chlorbutanol ,tetracycline,Oxytetracycline, Chlortetracycline, Nalidixic acid, Naproxen, Naproxen, Busulfan, Dipyrone

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Done by : Marwa Abd El Kader
Prelab 1
Alkalimetry (tab.) Bromometry (pd.) Std. Alkali Std. Br 2
1) Bromometry Aspirin NaOH, Boil C O O N a O H Salicylic acid Kn. Xss Std. Br2 COOH OH B r O H B rB r Tribromo phenol (TBP) yellow ppt I 2 Na2S2O3 Starch ind. NaOHHClStd. Br2 Decarboxilative bromination (as Br2 brominates phenolic cpds;thats why I changed aspirin to salicylic acid 5 ml CHCl3 with shaking
Here we have a solution of precisely weighed potassium iodate with added HCl that has just been served with an excess of potassium iodide. A disproportionation has occurred in the oxidation states of the iodine in iodate and iodide to produce elemental iodine complexed with the excess iodide to produce the triodide ion. A deep red-brown solution results (almost black) Iodate is titrated with thiosulfate solution in the process of standardizing it, the solution first turns a dark red, then orange, then yellow. Straw yellow color before adding the starch indicator.
Straw yellow colour
After adding starch Shake vigrously , e.p disappearance of blue colour
Volatile Toxic (sterility to males) Kn. Xss std KBrO3/KBr mix. Sample St. Br2 Conc. HCl
BrO3/Br Br2 Na salicylate Salicylic acid KI I2 Br2 / C. HCl Imp.
Interference Adsorption of Br2 & I2 on the surface No filtration Bec. I2 & Br2 are volatile Add CHCl3 or CCl4 Dissolves TBP
To the formation of the 1st strong complex with I2 We cant use bromometry in aspirin tablets assay ( as tab. contains starch as binder)
Calculations : Recovery % = Practical wt Theoretical wt X 100 ( Kn.xss*f mls Na2S2O3 *f) x F x D.F Kn xss 25 ml but bec. of its 24.8 ml Equivalent factor 1ml std . gm sample N.B. Most drugs recovery % = 95- 105 Whats done / whats taken Gm % W/W
C % = Practical wt Vol. X 100 Gm % W/V ? Std. ? Sample ( from balanced eq. , here in case of aspirin we can keep that it gave me 3 Br2 ) Conc. of std. F = N.B. Mole = M.wt on the balance Molar = Mole in 1 L
F = Std Sample 3 Br2 1 Aspirin 3M Br2 1M Aspirin 1M Br2 1/3M Aspirin M Br2 1M Aspirin 20 3x20 1ml M Br2 gm M.wt Aspirin 20 3x20x 1000 歎 3 We was working with M/20 Any no.s up write it here down Bel nazar ;)
C O O N a O H 2) Alkalimetry: Aspirin Kn. Xss std NaOH Std HCl NaOH + CH3COONa M/20 NaOH Boil gently Grind 2 tab.
Practical pharmaceutical chemistery
Identification Tests Aspirin pd + 4ml 2M NaOH + H2SO4 + FeCl3 dps Boil 1 min Salicylic Pd + 2ml Amm.molybdate Chloroquine + Trinitrophenol (picric)
Prelab 2 1) Isonicotinic acid Hydrazide (I.N.H) Bromometry (Redox) I.N.H Kn. Xss std. Br2 I 2 Na2S2O3 Starch ind. N/20 std Br2C. HCl Stand + 2 Br2 + H3O (oxidative cleavage) + + N2 +4 HBr Reducing agent
Any redox reaction needs acid as a catalyst . If the diluting solvent isnt mention, use H2O.
BrO3/Br Br I.N.H Oxidative Cleavage KI I2 Br2 / C. HCl Imp.
Calculations : The same idea as before :R%, C% & F No. of electrons gained or lost or no. of H or OH e.g. 1M H 2 SO4 = 2 N+
Identification Tests T.T 1 I.N.H pd +1ml H2O || T.T 2 2ml FehlingA+ 2ml Fehling B Red ppt (reduction of fehling)heat T.T 1 T.T 2
I.N.H pd +anh. Na2CO3 pyridine odour I.N.H pd + H2O Vanillin + H2O (conc. Soln.), heat With scratching - H2O Schiffs base N C O NH N CH OCH3 OH Yellow ppt
2) Chlorbutanol (Antimicrobial preservative):
Volhard's MethodMohr's MethodP.O.C Back (acidic medium)DirectType of Titration Std.1 (kn.xss): AgNO3 AgNO3Titrant Std.2 (titrant): NH4SCN Ferric ammonium sulfate (FeNH4(SO4)2) Potassium chromate ((K2Cr2O7 Indicator When all the chloride is converted to AgCl, the AgNO3 left is back titrated against std. NH4SCN ,the next excess of SCN reacts with the indicator and gives a red color ferrous thiocyanate (Fe(SCN)3) complex. When all the chloride existing in solution is completely precipitated as AgCl, the next excess drop of the titrant Ag chromate the color of the solution changes from yellow to a red ppt. At The End Point
Chlorobutanol heated with NaOH (To transform the organic aliphatic halide to inorganic one) 3 NaCl Chlorobutanol Kn. Xss AgNO3 Isopropanol Dil. HNO3 AgCl NH4SCN Ferric allum ind. NaCl+ AgNO3 AgCl + NaNO3 AgNO3 + NH4SCN AgSCN+ NH4NO3 NH4SCN+ FeNH4(SO4)2 [Fe(SCN)3] + 2 (NH4)2SO4
e.p white ppt in a buff solution
1 is Unsuccessful & always dissociating called AgCl ( Ksp) 1 is successful,respected & always relaxed & at ease called AgSCN ( Ksp)
If the problem is with the dissociated Ag ions of the AgCl, we must get rid of that AgCl , mmm boiling& filtration well not work well as coagulation of ppt will occur , thus dec. the S.A ,so why not to coat them & cross them over as if well do that to act like a bridge in order not to fall down & get stuck in that tight corner?! But How ?!!! Ahha, I knew ,Ill use Isopropanol or nitrobenzene ;) +
Ksp AgCl > Ksp AgSCN Ksp AgI,AgBr < AgSCN To ensure no alkalinity AgNO3 AgOH AgO2 (black ppt.) Fe 3+ Fe(OH)3 OH OH
Calculations : The same idea as before :R%, C% & F AgNO3 =Chlorbutanol= 3NaCl Cyclophosphamide & Enteroquine have the same principle
Identification Tests Oxytetracycline Chlortetracyclinetetracycline Pd + 1ml conc. H2SO4 [dehydration inc. conj. color] {tautomerism} Deep crimson red (violet) Red (pink) color Deep blue to green color + FeCl3 Brown color (phenolic cmpd)
Prelab 3 Bu sulfanNaproxenNaproxenNalidixic acid P.O.C Direct AFTER HYDROLYSIS 2 Me sulfonic acid DirectDirectBack (due to intramolecular H- bond & Zwitter ion formation non polar insol. in H2O,slightly sol. In alc.) Type of Titration NoYes, as naproxen but till 250ml Yes(H2O [all at once], alc. till 100 [ shwaya b shwaya) NoDilution M/20 NaOHM/20 NaOHM/40 NaOHStd. acid (we havent worked it in lab) Titrant Acid Base Titration
Calculations : The same idea as before :R%, C% & F Given as each 1 ml 0.1M NaOH is 23.03 mg naproxen ,since we worked with M/40 , so weve to divide this value by 4 We dont have M/40 in lab , so well dil. M/20 to M/40 50ml NaOH M/20 + 50ml H2O M/40 2 NaOH = Busulfan 2
Identification Tests Pd = 2ml conc. HCl + 0.5ml Soln. 硫 naphthol in alc. orange red ppt Charge transfer complex Electron rich Electron poor
Pd. + 2ml H2O + 1ml conc. H2SO4 + 0.2 gm vanillin yellow to orange pptBoil - H2O Conj. Compound (orange ppt.) Dehydrating agent is H2SO4 Active methylene easy to liberate OH
Giriseofulvin: Pd + 2ml conc. H2SO4 + few K2Cr2O7 Red color Oxid. reaction Quinoid str. (color)
Prelab 4 1) Dipyrone Dipyrone + distilled H2O 1ml glacial acetic acid N/10 I2 +I2 +HI + NaHSO4 CH2 Rose red color (Dimer)
Identification Tests Dipyrone pd +10ml dist. H2O 2ml +2ml dil. HCl Odour of SO2 Odour of formaldehyde +1.5 ml dil. HCl +1ml FeCl3 bluered color disappear + 1ml K- pyronantimonate white ppt.
http://www.csudh.edu/oliver/demos/hh- cubr/hh-cubr.htm http://www.edu.xunta.es/centros/iesbreamo/ galeria/displayimage.php?album=141&pos=15 Read more: Precipitation Titration Techniques | eHow.com http://www.ehow.com/info_8665193_precipitation- titration-techniques.html#ixzz2PiURhefH

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Practical pharmaceutical chemistery

  • 1. Done by : Marwa Abd El Kader
  • 4. 1) Bromometry Aspirin NaOH, Boil C O O N a O H Salicylic acid Kn. Xss Std. Br2 COOH OH B r O H B rB r Tribromo phenol (TBP) yellow ppt I 2 Na2S2O3 Starch ind. NaOHHClStd. Br2 Decarboxilative bromination (as Br2 brominates phenolic cpds;thats why I changed aspirin to salicylic acid 5 ml CHCl3 with shaking
  • 5. Here we have a solution of precisely weighed potassium iodate with added HCl that has just been served with an excess of potassium iodide. A disproportionation has occurred in the oxidation states of the iodine in iodate and iodide to produce elemental iodine complexed with the excess iodide to produce the triodide ion. A deep red-brown solution results (almost black) Iodate is titrated with thiosulfate solution in the process of standardizing it, the solution first turns a dark red, then orange, then yellow. Straw yellow color before adding the starch indicator.
  • 7. After adding starch Shake vigrously , e.p disappearance of blue colour
  • 8. Volatile Toxic (sterility to males) Kn. Xss std KBrO3/KBr mix. Sample St. Br2 Conc. HCl
  • 10. Interference Adsorption of Br2 & I2 on the surface No filtration Bec. I2 & Br2 are volatile Add CHCl3 or CCl4 Dissolves TBP
  • 11. To the formation of the 1st strong complex with I2 We cant use bromometry in aspirin tablets assay ( as tab. contains starch as binder)
  • 12. Calculations : Recovery % = Practical wt Theoretical wt X 100 ( Kn.xss*f mls Na2S2O3 *f) x F x D.F Kn xss 25 ml but bec. of its 24.8 ml Equivalent factor 1ml std . gm sample N.B. Most drugs recovery % = 95- 105 Whats done / whats taken Gm % W/W
  • 13. C % = Practical wt Vol. X 100 Gm % W/V ? Std. ? Sample ( from balanced eq. , here in case of aspirin we can keep that it gave me 3 Br2 ) Conc. of std. F = N.B. Mole = M.wt on the balance Molar = Mole in 1 L
  • 14. F = Std Sample 3 Br2 1 Aspirin 3M Br2 1M Aspirin 1M Br2 1/3M Aspirin M Br2 1M Aspirin 20 3x20 1ml M Br2 gm M.wt Aspirin 20 3x20x 1000 歎 3 We was working with M/20 Any no.s up write it here down Bel nazar ;)
  • 15. C O O N a O H 2) Alkalimetry: Aspirin Kn. Xss std NaOH Std HCl NaOH + CH3COONa M/20 NaOH Boil gently Grind 2 tab.
  • 17. Identification Tests Aspirin pd + 4ml 2M NaOH + H2SO4 + FeCl3 dps Boil 1 min Salicylic Pd + 2ml Amm.molybdate Chloroquine + Trinitrophenol (picric)
  • 18. Prelab 2 1) Isonicotinic acid Hydrazide (I.N.H) Bromometry (Redox) I.N.H Kn. Xss std. Br2 I 2 Na2S2O3 Starch ind. N/20 std Br2C. HCl Stand + 2 Br2 + H3O (oxidative cleavage) + + N2 +4 HBr Reducing agent
  • 19. Any redox reaction needs acid as a catalyst . If the diluting solvent isnt mention, use H2O.
  • 21. Calculations : The same idea as before :R%, C% & F No. of electrons gained or lost or no. of H or OH e.g. 1M H 2 SO4 = 2 N+
  • 22. Identification Tests T.T 1 I.N.H pd +1ml H2O || T.T 2 2ml FehlingA+ 2ml Fehling B Red ppt (reduction of fehling)heat T.T 1 T.T 2
  • 23. I.N.H pd +anh. Na2CO3 pyridine odour I.N.H pd + H2O Vanillin + H2O (conc. Soln.), heat With scratching - H2O Schiffs base N C O NH N CH OCH3 OH Yellow ppt
  • 25. Volhard's MethodMohr's MethodP.O.C Back (acidic medium)DirectType of Titration Std.1 (kn.xss): AgNO3 AgNO3Titrant Std.2 (titrant): NH4SCN Ferric ammonium sulfate (FeNH4(SO4)2) Potassium chromate ((K2Cr2O7 Indicator When all the chloride is converted to AgCl, the AgNO3 left is back titrated against std. NH4SCN ,the next excess of SCN reacts with the indicator and gives a red color ferrous thiocyanate (Fe(SCN)3) complex. When all the chloride existing in solution is completely precipitated as AgCl, the next excess drop of the titrant Ag chromate the color of the solution changes from yellow to a red ppt. At The End Point
  • 26. Chlorobutanol heated with NaOH (To transform the organic aliphatic halide to inorganic one) 3 NaCl Chlorobutanol Kn. Xss AgNO3 Isopropanol Dil. HNO3 AgCl NH4SCN Ferric allum ind. NaCl+ AgNO3 AgCl + NaNO3 AgNO3 + NH4SCN AgSCN+ NH4NO3 NH4SCN+ FeNH4(SO4)2 [Fe(SCN)3] + 2 (NH4)2SO4
  • 27. e.p white ppt in a buff solution
  • 28. 1 is Unsuccessful & always dissociating called AgCl ( Ksp) 1 is successful,respected & always relaxed & at ease called AgSCN ( Ksp)
  • 29. If the problem is with the dissociated Ag ions of the AgCl, we must get rid of that AgCl , mmm boiling& filtration well not work well as coagulation of ppt will occur , thus dec. the S.A ,so why not to coat them & cross them over as if well do that to act like a bridge in order not to fall down & get stuck in that tight corner?! But How ?!!! Ahha, I knew ,Ill use Isopropanol or nitrobenzene ;) +
  • 30. Ksp AgCl > Ksp AgSCN Ksp AgI,AgBr < AgSCN To ensure no alkalinity AgNO3 AgOH AgO2 (black ppt.) Fe 3+ Fe(OH)3 OH OH
  • 31. Calculations : The same idea as before :R%, C% & F AgNO3 =Chlorbutanol= 3NaCl Cyclophosphamide & Enteroquine have the same principle
  • 32. Identification Tests Oxytetracycline Chlortetracyclinetetracycline Pd + 1ml conc. H2SO4 [dehydration inc. conj. color] {tautomerism} Deep crimson red (violet) Red (pink) color Deep blue to green color + FeCl3 Brown color (phenolic cmpd)
  • 33. Prelab 3 Bu sulfanNaproxenNaproxenNalidixic acid P.O.C Direct AFTER HYDROLYSIS 2 Me sulfonic acid DirectDirectBack (due to intramolecular H- bond & Zwitter ion formation non polar insol. in H2O,slightly sol. In alc.) Type of Titration NoYes, as naproxen but till 250ml Yes(H2O [all at once], alc. till 100 [ shwaya b shwaya) NoDilution M/20 NaOHM/20 NaOHM/40 NaOHStd. acid (we havent worked it in lab) Titrant Acid Base Titration
  • 34. Calculations : The same idea as before :R%, C% & F Given as each 1 ml 0.1M NaOH is 23.03 mg naproxen ,since we worked with M/40 , so weve to divide this value by 4 We dont have M/40 in lab , so well dil. M/20 to M/40 50ml NaOH M/20 + 50ml H2O M/40 2 NaOH = Busulfan 2
  • 35. Identification Tests Pd = 2ml conc. HCl + 0.5ml Soln. 硫 naphthol in alc. orange red ppt Charge transfer complex Electron rich Electron poor
  • 36. Pd. + 2ml H2O + 1ml conc. H2SO4 + 0.2 gm vanillin yellow to orange pptBoil - H2O Conj. Compound (orange ppt.) Dehydrating agent is H2SO4 Active methylene easy to liberate OH
  • 37. Giriseofulvin: Pd + 2ml conc. H2SO4 + few K2Cr2O7 Red color Oxid. reaction Quinoid str. (color)
  • 38. Prelab 4 1) Dipyrone Dipyrone + distilled H2O 1ml glacial acetic acid N/10 I2 +I2 +HI + NaHSO4 CH2 Rose red color (Dimer)
  • 39. Identification Tests Dipyrone pd +10ml dist. H2O 2ml +2ml dil. HCl Odour of SO2 Odour of formaldehyde +1.5 ml dil. HCl +1ml FeCl3 bluered color disappear + 1ml K- pyronantimonate white ppt.
  • 40. http://www.csudh.edu/oliver/demos/hh- cubr/hh-cubr.htm http://www.edu.xunta.es/centros/iesbreamo/ galeria/displayimage.php?album=141&pos=15 Read more: Precipitation Titration Techniques | eHow.com http://www.ehow.com/info_8665193_precipitation- titration-techniques.html#ixzz2PiURhefH