- Exercises Draw The Structures Of The Complexes Prepared In Parts B And C Consult The Ir Spectra Obtained Given That 1 (21.98 KiB) Viewed 53 times
- Exercises Draw The Structures Of The Complexes Prepared In Parts B And C Consult The Ir Spectra Obtained Given That 2 (22.41 KiB) Viewed 53 times
- Exercises Draw The Structures Of The Complexes Prepared In Parts B And C Consult The Ir Spectra Obtained Given That 3 (29.18 KiB) Viewed 53 times
- Exercises Draw The Structures Of The Complexes Prepared In Parts B And C Consult The Ir Spectra Obtained Given That 4 (25.93 KiB) Viewed 53 times
- Exercises Draw The Structures Of The Complexes Prepared In Parts B And C Consult The Ir Spectra Obtained Given That 5 (62.74 KiB) Viewed 53 times
- Exercises Draw The Structures Of The Complexes Prepared In Parts B And C Consult The Ir Spectra Obtained Given That 6 (60.9 KiB) Viewed 53 times
www Analy Date CHEMU Today 26, 2016 PM 54 50 YT 45 2015 m. 225T 40 35 soos 5.50 4T 30 T 1,24 54 se 25 20 3436cm Noth band ملهمها 15 1594cm 10 450 5 1500 1000 4000 21 Odom-1.91T 2924 Som-1.435T 3289150 2500 2000 cm-1 12.66%T Sample 005 By CHEM User Date Tuesday, October 20 2021 3500
Analyst CHEMU Tuesday, October 26, 2021 11:50 AM Date 2 Oro 3231192 1357 0.254 3149SORAT 100.355 14633 5441526 to 1. VERWANT 37 USO SNOST 40 38 36 34 32 3640 mm. an. 30 28 26 24 22 20 2 2043 3114 OTOT 300DT 2650 2002 1994 tom.27 142136am-1.27239 To Stom:1. 25.67% %T d 24 25.50T Buuhani الہ سے 7 band 1638 un 18 16 14 1000 450 12 16376cm-1, 11.51% 11 4000 3500 312891,60 2500 2000 1500 cm-1 CHEM User 021 34 21 %T Sample 002 BY CHEM User Date Tuesday, October 26 2021
CHEMU Tuesday, October 26, 2021 12:03 PM Analyst Dale 75 70 secondary SW rpm 05 13 m. 15TBANT 60 55 1922 1941 50 45 40 3431 om 1,40T %T 35 30 N77.0.1.30. 20% 25 امید است - 20 Najol. 1400 35cm., 18.94%T zhat 15 TO 1500 1000 450 5 233331549 -0 2011.4305 4000 3500 32891.69 2500 2000 cm-1 samplec 7.73 %T Sample 003 By CHEM User Date Tuesday, October 26 2021
om OLA c) A nickel(II) complex with 1,2-diaminopropane and pyrrole-2-aldehyde equipped with a twin-necked adaptor, reflux condenser and dropping funnel. Place In the designated fume cupboard, set up a round-bottomed "Quickfit" flask (100 cthanol-water mixture (1:1 wv, 50 cm) in the flask along with pyrrole-2-aldehyd (0.95 g), nickel ethanoate (nickel acetate, Ni(OCOCH3)2-4H20, 1.25 g) and 3 anti-bumping granules. Heat the flask to dissolve the nickel ethanoate (a turbid raket than clear solution will form) and then add an aqueous solution of NaOH (10% wlv, refluxing suspension of nickel hydroxide and aldehyde. Next, add water (10 cm) Add this diamine solution dropwise, over a period of about 20 minutes, to live cm'). Dissolve 1,2-diaminopropane (0.4 cm') in water (20 cm') in the dropping fuel with a little ethanol-water (1:1). Redissolve the product in dichloromethane (ca. 40 allow the mixture to cool. Collect the crude orange product by filtration and was cm') while still in the filter funnel and allow the orange dichloromethane solution magnesium sulfate, remove the magnesium sulfate by filtration and wash the filter into a clean conical flask (100 cm'). Dry this solution with a little anhydrous magnesium sulfate with a little dichloromethane. Add light-petroleum (80-100°C) evaporator. (Use a room temperature water bath and do not heat the flask). The orange the combined filtrate and washings, and remove the dichloromethane using a product will precipitate from the light-petroleum as the dichloromethane is removed and may then be collected by filtration and allowed to dry in air. Record your yield VS rotary and obtain the IR (KBr disc), 'H NMR and mass spectra of your product.
the following experiments, nickel complexes of two isomeric ligands derived from NMR, MS and IR spectral measurements can be used to investigate the structures of diaminopropane and pyrrole-2-aldehyde are prepared using different methods. 'H these compounds Experimental a) A Schiff base ligand from 1,3-diaminopropane and pyrrole-2-aldehyde "This reaction is to be carried out in the designated fume cupboard. Dissolve pyrrole-2- aldehyde (0.95 g) in ethanol (5 cm) in a round-bottomed "Quickfit flask (100 cm). a graduated pipette, add 1,3-diaminopropane (0.40 cm) to the solution and mix Using the liquids. Fit a reflux condenser and warm the flask and tellux for 3-4 min and then stand in an ice bath for 2 hours. The mixture may solidify to a crysulline mission remain liquid. If a solid has deposited on cooling collect this by filtration and wash it with a few cm' of cold EtOH. The combined filtrate and washing may deposit more products, as crystalline needles, on standing. If the mixture remains liquid, reduce the volume on a rotary evaporator, until solid starts to appear and then stand the task in an ice bath to complete the crystallization. Proceed to collect the product as described above. Allow the product to air dry and record your yield. Obtain the IR (KBr disc), 'H NMR and mass spectra of your product. b) A nickel(II) complex form the Schiff base ligand Dissolve a portion (0.5 g) of the ligand prepared above in a) in warm ethanol (10 cm) Slowly add a solution of nickel ethanoate (nickel acetate, Ni(OCOCH3)2-4H20,0.58 in water (10 cm) to produce a turbid, brick red mixture. Next add a solution of sodium carbonate (0.2 g) in water (5 cm) and stir the mixture for 20 minutes. After this time, collect the crude product by filtration and wash it with a little ethanol-water mixture (1:1, a few cm). Redissolve the red product in dichloromethane (ca. 40 cm) and dry the solution over a little anhydrous magnesium sulfate. Remove the magnesium sulfate by filtration and wash it with a little dichloromethane. Add light- petroleum (80-100°C, 40 cm) to the combined washings and filtrate, then remove the dichloromethane using a rotary evaporator (use a room temperature water bath, do not heat the flask). The red product will precipitate from the light petroleum as the dichloromethane is removed. The product may be collected by filtration and air dried Record your yield and obtain the IR (KBr disc), 'H NMR and mass spectra of your product