Question

I need to make a flowchart for this procedure but I am not sure how to guide myself.

Experimental Method 1. Place a stir bar in a 100 ml. RB flask filled with a lisen adapter and a reflux condenser, and then d-bromancelephence (1000 ml) photos acid (0.69 55 mmol) and 1-propanol 10 mLbp 97 °C). Stir the mixture for 15 min under a slow flow of nitrogen gas going into the Claisen adaptor side arm e a budes attached to the top of the condenser to observe the flow), to llow the complete dissolution of the solids 2. Briefly raise the condenser up and the timing w palladium acetate (4 mg. 16 umol). eriphenylphosphine (13 mg, Soumoll The M u s eum carbonate (3.25 ml. 65 mmol). and distilled water (20 mL) in the same way. Continue flushing with nitrogen for a few more minutes, then replace the nitrogen Bow with a nitrogen hallen, as demonstrated by your TA. 3. Heat the reaction mixture to reflux under the nitrogen environment for at least 1 h. Observe any color changes . then stif 4. Cool the reaction flask to room temperature remove the case and add water the mixture open to the air for 5 min. 5. Extract the aqueous layer with ethyl acetat (2 x 10 ml.). Then combine the organic extracts and wash them with 5 sodium bicarbonate solution (2 x 10 mL) and saturated sodium chloride solution (brine) (2 x 10 mL). 6. Transfer the organic layer to a 125 ml. Erlenmeyer flask and add decolonizing charcoal (0.50 g) and sodium sulfate ( ). Stir for 10 min., then vacuum filter through a 1 cm bed of Celite, using a Buchner funnel. Rinse the Celite with several small portions of ethyl acetate, then evaporate the filtrate down to dryness using a rotory evaporator Report the crude yield of your product 7. Recrystallisation and analysis (may be done the following week). Recrystallize your crude product from hexames (about 5 ml) and a small quantity of methanol. To do this, gently warm the slurry formed by adding the hexes to your product until it is to bear the boiling point. Then add just enough methanol to clarify the solution. Remove the solution from the heat source, and allow it to cool slowly Collect the crystalline product and report the yield. Also, analyze the product by TUC (developed in 4:1 hexanes: ethyl acetale), melting point and when directed to do so) proton NMR Assign the peaks in he proton NMR as completely as you can and report any observable cevapling constants

I was given this procedure which is for Suzuki-Cross Coupling Reactiob: Synthesis of 4 - acetylbiphenyl, and I need to make a flowchart. I need help with that.

Answer 1

0.690 Weigh loog of u-Bromo acetophenone, onic acid and measure lome of 1-propand and add in RB flask / Stir for 15 minutes under La flow. Add uing of Palladium acetate, 13 ing of triphenylphosphine followed by 2M sodium Carbonate and 2.om. distilled water I continue Nitrogen flushing & for 5 mins. Then Replace I with Nitrogen balloon. Heat to Reflux for Ihrunder Nitrogen! environment to Room temperature Add Tome of water and ster the I mixture open to arr for smins. { Extract aqueous layer with ethyl acetate twice (10ml each time). rcombine ethyl acetate layer and wash with 5%. Natio, twice (loml each time). then with saturated Nace solution (twice)

Decolorize organic layer with activated charcoal (0.50g) and Sodium sulfate (1.00 g) leptomas. Stir for 10 min. I vacuum filter the contents over Celine Evaporate soment using rotary ] gh crude product The Recrystallize using hexane and small amount of methanol Analyze the product by TLC and spectral studies