With the official start of summer research, we jumped right in and synthesis started the second day. The first step in the reaction pathway is the addition of a dithiol to synthesize a substitutated dithiane. The dithiane acts as a protecting group through the next step and is finally removed during the final reaction. In other words, we work with sulfur, a lot. This means that our lab and clothes commonly smell like sulfur all day and an extra shower is essential. It may be gross, but it is a necessary step that allows us to do fun chemistry.
More recently, we have been focusing on the palladium catalysis reactions. For these time monitoring reactions of the synthesis of benzophenones, the sample is prepared in a dry box. Since I work for a relatively new lab, we are often privileged to have the latest equipment. However, as the glovebox was new and not one hundred percent set up, we encountered a few hiccups. After it was finally set up, we noticed that one of the bolts did not fit properly. Therefore, a few days had to go by before it could be shipped, received and attached. None-the-less, the dry box is now functional and a beautiful piece of equipment, in both looks and function. When the lights in the room are off and the glovebox lights are on, it glows with pristine cleanness. With regards to function, it allows chemistry to be done without exposure to air, meaning no water and limited O2.
For the past few days, I have been excited to be working in the dry box. With my arms encased in thick plastic gloves, I resemble a robot and often get weird stares from the hallway. Perhaps they are intrigued or maybe they are just confused. As one can imagine, plastic gloves are not always pleasant in the hot summer months; however, I was thrilled to start monitoring reactions. In order to properly monitor these reactions, an internal standard must be introduced prior to the start of the reaction. This allows for calibration and for the amount of starting material and product present to be compared among many time points. With my first reaction, I forgot to add biphenyl (the internal standard). Mistakes make great lessons though and I am certain it will not happen again. This little accident has made me more meticulous in making sure everything is within the microwave vial before removing it from the dry box. Now, the goal is to complete and repeat, multiple times.