Synthesis of Pd(0) catalyst tetrakistriphenylphosphinepalladium | Quick guide

Hello my dear chemists! :D Sorry that isn't 4K, I am fixing my tech. FULL TEXT Today I am gonna show you how to make a tetrakistriphenylphosphinepalladium (0). This substance is a widespread catalyst for most of organic reactions including Stille, Sonogashira, Suzuki-Miyara coupling reaction, generally those require source of palladium species dispersed in reaction mixture. First of all we need a Schlenk flask with 50 ml of fresh dimethylsulfoxide. Next it needs to be aerated by argon during 20 min. For this purpose, I use a balloon equipped with a long adrenaline needle. After time is gone I put 3 grams of triphenylphosphine and 0.5 grams of palladium dichloride then stirring reaction mixture till 5 minutes until the presence of yellowish color. Further funnel is removed and flask is covered by rubber septum gently to prevent reaction mixture from air and moisture. To prompt a reaction, we need all compounds to be solvated so it should be heated up to 140 – 160 degrees C. For this procedure I am gonna use a silicon oil bath, of course controlling temperature. As you can see, right solution is transparent and looks like whiskey. So now we need to activate complexation of Pd(0) by adding 0.5 ml of hydrazine hydrate through the septum. Solution become instantly darker because of palladium black nanoparticles and fumes of ammonium chloride could be seen. Now just turn off the hotplate and let it cool down overnight with stirring. After temperature down below 140 degress C nice flakes of tetrakis are coming out. On the next day whole precipitate releases and ready to be filtered off under inert atmosphere. Due to my grinding poverty I use system presented on screen, of course you could use a Schlenk line or glove box. Tetrakis should be filtered and washed three times with 15 ml portions of methanol and same with diethyl ether. Please mention in comment section if you like to know the principle of operation for my filtering system. Clean product should be between yellow and grey color and has strong green fluorescence. In my case the final yield is 2.81 g that about 86%. ------------------------------------------------------------------- Socials: ► Support me on PayPal: https://paypal.me/acantharex Music: 1) Abstrakt - Nobody Else [NCS Release] -------------------------------------------------------------------- Tags: #chemistry #palladium #complex #guide #science #acantharex #organicchemistry chemistry, organic chemistry, guide, tutorial, experiment, fluorescence, solid state, evaporation, inorganic chemistry, laboratory equipment, science, routine procedures, how to, palladium metal, Pd[PPh3]4