To a solution of substituted chloro quinoxaline compound (2a) (4.5g, 12.9 mmol) weighed into a round bottom flask was charged with PdCl2 (dppf).DCM (6%mol, 0.633g). A toluene: ethanol mixture in 2:1 ratio (40 ml+20 mL) was degassed with nitrogen gas, and then added into the flask. Aqueous 1 molar sodium bicarbonate solution (24 mL, 19.30 mmol) was degassed and added to the mixture. The mixture was stirred at room temprature for 15 minutes under nitrogen. The 3-methyl phenyl boronic acid (2.1 g, 15.48 mmol) or respective boronic acid (2-methoxy phenyl boronic acid/ 3-methoxy phenyl boronic acid/ 2-fluoro boronic acid) was added as the solid. The reaction was refluxed under nitrogen gas for overnight and completion was checked by the TLC (Ethylacetate: hexane; 2:3). The reaction mass was cooled to RT. Then the solvent was completely evaporated under reduced pressure. Obtained a black colored product. It was purified by silica column chromatography (10:90 ethyl acetate: hexane) to get the compound (3a-d) …show more content…
TFA (4 times w/v, 18 mL) was slowly added and stirred for 4-6 hours at room temperature. The reaction was monitored by HPLC-MS and TLC. When the reaction was complete, the solvent was concentrated in vacuo; methanol was added (2×50 mL) and evaporated in vacuo. The product was dissolved in methanol and basified with 7N ammonia in methanol. The solvent was concentrated in vacuo and the product was dissolved in methanol (70mL). micro porous tosic acid (MP-TSOH) (12.93 g, 42.83 mmol) was added and the reaction mixture shaken at room temperature for overnight. The resin was washed with methanol, and cleaved with 2N NH3 in methanol. The solvent was evaporated to get the free based compound
It was made basic by adding 6 mL of 6M NaOH to the separatory funnel. The pH was taken to confirm that it was basic. Next, 10 mL of dichloromethane was added to the flask. The flask was shaken and the bottom layer was drained in a flask. This was repeated two more times. Na2SO4 was added to the flask to remove water. A flask was pre-weighed and gravity filtration was conducted. After, a TLC was conducted for p-toluidine and there was only one spot on the plate with an Rf of 0.32. Then a boiling stick was added to the flask and was placed on sand bath to completely boil. The weight of the flask was taken again.
Furthermore, the principles and metrics of green chemistry were incorporated into the synthesis reaction through the use of the benign solvent, water. Through the use of the vacuum filtration and the recrystallization procedures, the product was further purified. Subsequently, the purity and identity of the product were evaluated through the analysis tool of Nuclear Magnetic Resonance. Ultimately, the efficiency and greenness of the reaction were measured through the calculation of the percent yield and the atom
This week in lab we focused on reducing Ketones to Secondary Alcohol’s. Hydride reducing agents such as LiAlH4 and NaBH4 react with ketones to produce 2o alcohol. In our experiments, we used NaBH4 as it is a milder reducing agent and can be used in protic solvents such as ethanol. The first week a reaction was carried out using 9-fluorenone as the ketone. And the second my group and I used a variety of ketones to see how they reacted differently.
In this experiment, the reduction of 4-tert¬-butylcyclohaxanone was performed using sodium borohydride. To complete this reduction, 0.5010 g of 4-tert¬-butylcyclohaxanone was added to 6.0 mL of methanol and heated until the ketone dissolved completely. Next, 0.0510 g of sodium borohydride was added to the solution. At this time, bubbles formed and an exothermic reaction took place. After the solution was stirred for 20 minutes, 2 mL of sulfuric acid was added to the flask. The solution became white and cloudy, and more bubbles formed. Immediately after the acid was added, 5 mL of water was also put into the reaction flask. The solution was stirred for 10 minutes. During this time, a white solid formed. After this, the solution was
Function: The function of this product is to reduce underarm wetness and control body odor. The deodorant aspect of this product reduces body odor by killing the odor-causing bacteria. The antiperspirant aspect of this product mitigates wetness by inhibiting gland sweat.
A simple, rapid, sensitive and effective reverse phase ultra performance liquid chromatographic method (RP-UPLC) has been developed and validated an assay for simultaneous quantification of Lamivudine, Abacavir and Dolutegravir in pure and tablet dosage forms. Chromatographic separation was performed by using Waters- Alliance UPLC system equipped with autosampler, PDA detector, zodiac sil RP C18 (4.6×250mm 3.0µm) column, phosphate buffer (pH 3.0) and methanol in the ratio of 30:70 v/v have been delivered at a flow rate of 0.25 mL/min and the detection was carried out using a UV detector at a wavelength 260nm at ambient column temperature. The mobile phase is used as diluent. The retention time (Rt) for Lamivudine, Abacavir and Dolutegravir
Label three test tubes A - C and place them in a test tube rack. Using a graduated beral-type pipet and add about 2 mL of the cobalt chloride solution to each test tube A - C. Make sure a pipet is used to measure so that all volumes are equal. Place A in an ice bath, B in boiling water, and C should remain a constant temperature. Add HCl to each and observe.
When the PKCγ-Cγ3 images are viewed separately, in the trials with the constitutively active PLCγ1 (A25E) mutant positive control, we will see the PKCγ (indicated by the pink color of Cγ3) move closer to the edges of the cell (which are defined by phase microscopy). In the same trials, the fascin-FTIC images will show the location a fascin to be near the edges of the cell as well (as indicated by the green FTIC). Once these two images are layered over one another, will show an overlap of the to colors. A closer inspection of the edges and protrusions of the cell in this image, we should see both PKCγ and fascin in high concentrations right along the membrane.
1. Enzymes are protein molecules that act as catalysts in chemical reactions. These protein catalysts will speed up biochemical reactions in the body without being consumed in the process.
Starting reactants ethyl 4-bromobutyrate (5.85 g, 30 mmol) and sodium azide (2.925 g, 45 mmol) was added into dimethyl sulfoxide (DMSO, 20 mL) with stirring. The reaction mixture was stirred for 22 h at 55 °C, and cooled to room temperature. Water was added to the reaction mixture and extracted three times with 30 mL of ethyl ether. The combined organic layer was washed with water and brine, and rotary evaporator was used to remove the organic solvent and yield 3.67 g of the azido compound 1.
7 screw cap test tubes were labeled as 0µmol/L, 1.5µmol/L, 2.5µmol/L, 3.5µmol/L, 4.5µmol/L, 5.5µmol/L and 6.5µmol/L. Then, 0µL, 75µL, 125µL, 175µL, 225µL, 275µL and 325µL volume of 0.1mM MDA stock solution was orderly added into screw cap test tubes. 2.0mL of 1% TBA was added into screw cap test tubes. Distilled water was added into screw cap test tubes until total volume reached 5.0mL. They were mixed on whirl mixer. Then, they were wormed on a block heater at 100˚c for 30 minutes. After, they were allowed to cool in cold water for 5minutes. 7 centrifuged tubes were labeled as 0µmol/L, 1.5µmol/L, 2.5µmol/L, 3.5µmol/L, 4.5µmol/L, 5.5µmol/L and 6.5µmol/L. Then, the contents were orderly transferred to centrifuge tubes. They were centrifuged
A flea stir bar and 4.0 mL of 95% ethanol were added to the microwave reactor vessel. The solution was then stirred using a magnetic stirrer until all the KOH dissolved. 1.0 g of meso-stilbene dibromide was added in the microwave reactor vessel. The cap of the vessel was placed, tightened and the vessel was placed in a microwave reactor carousel. After the reaction was complete, the vessel with the mixed reaction was placed in a tap water bath so that it may be cooled. After it cooled down, 10 mL of DI water was placed in a 50 mL and the reaction mixture was poured into there to precipitate the product. The product was then collected by vacuum filtration and Hirsch funnel. The product was rinsed with 3 mL of DI water three times. The product dried on the filter paper with the vacuum on for 5 minutes after the rinse. The product was then placed in a drawer so that it may completely dry so that the weight and the melting point may be recorded later. The final product was a light brown
To a 5 mL conical vial with a spin vane, 5-nitro-2, 3-dihydrophthalazine-1, 4-dione (.151 grams) was added. Next, sodium hydroxide (2 mL, 3M) was added to the conical vial and stirred until a reddish brown color was obtained. The addition of sodium hydrosulfite (.254 grams) followed, and the sides of the conical vial were
The chemical formula for sodium hydroxide is NaOH. It has a ph of 11 and is considered as a base. The chemical formula for hydrochloric acid is HCl and it has a ph of 2 and is considered as an acid. The chemical formula of ammonia is NH3 and it has a ph of 8 and is considered as a base. The chemical formula of sodium chloride is NaCl and it has a ph of 7 and is considered aa a base. The chemical formula for deionized water is H2O and has a ph of 7 and is considered neutral. The 7up had a ph of 3 and is considered as an acid. The Maalox had a ph of 8 and is considered as a base. The apple juice had a ph of 4 and is considered as an acid. The vinegar had a ph of 2 and is considered as an acid. When it comes to the color of the indicator in
All the reagents used in this work were of AR grade chemicals and were used without further purification. Distilled water was used for washing all glassware and preparing solutions. The solid phase used is potassium Zinc hexacyanoferrate ion exchange.