Week 5 was a lot more of finding my independence within the lab. Johnny would plan out the reactions within his notebook, then we would set them up together, and then I would check up on them throughout the day and do the required purification processes. Overall, it was a super busy week and I had a great time.
Monday was a slower day as we had no reactions running over the weekend, so we basically had to start everything from scratch. I spent the morning waiting for Johnny to figure out what reactions we were going to run. After he found the reactions he wanted and set it all up within his online notebook, we measured out the substrate, salt, solvent, and catalyst. We set up two reactions and left them to run. A bit later I TLC’s the two reactions to see if they had finished or not, one was done and one wasn’t. I then did an acid workup on the reaction to neutralize it and purify. I added hydrochloric acid to the reaction and then extracted it using a separatory funnel.
On Tuesday, things started to pick up. I started the day by TLC ing the incomplete reaction from monday and it still wasn’t complete. Along with this, I finished the purification process from the complete reactions from the previous day by rotovapping it down to get all the solvent off, so we just had the product left. Me and Johnny then set up 2 reactions that had this super smelly chemical in it that would prove to be a huge challenge in the coming days.
Wednesday, I started the day by TLC ing the two reactions from the previous day and they were both complete, so we ran base work ups on them. Johnny then left me the task of rotovapping both reactions down, as he had a meeting that he had to go to. This normally would’ve been fine, but due to the smelly chemical being in there, when I took the flask off the rotovap, the small concentrated oil smelled up the whole lab. Everyone ditched their fume hoods and work spaces to go to their closed off office spaces or out of the lab in whole. I didn’t really know what to do, but luckily Amit helped me out and we got everything closed off in a fume hood. Right as it all reached its peak, Johnny returned to the aftermath and he dealt with the source as I febreezed down the whole lab. After this, we were very careful to keep these substances in the fume hood at all times or in isolated areas.
Thursday was spent using the biotage for these two reactions to further purify them. To load them into the biotage, I mixed our substance with silica powder and then loaded each into their own cartridge. Johnny then hooked them up to the machine and we got our vials of product. I then TLC’d the viles to see where our product was, poured them into a flask, and rotovapped it down until we reduced from 500 ml of liquid to a couple ml of pure product. I did this three different times just for the first reaction as we got three different materials out of the separation from the biotage. By this time the smell was mostly gone so I didn’t have to worry about it too much. Johnny then took care of the second.
Friday was mostly spent on clean up, setting reactions to run over the weekend, and NMR. I washed out all the flasks and funnels we used over the course of the week with soap, water, and acetone. Throughout the day, me and Johnny had reserved NMR time to see if we got what we wanted in our reactions. Turns out in the really stinky stuff that caused so much problem, we didn’t get what we wanted, so essentially did all that for nothing. Since it was Friday, we also had group meeting which most attended by zoom since Keary wasn’t there. We then finished the day by setting up four reactions. Notably, one of which used nitric acid, pretty gnarly stuff.
Other then the lab, Saturday was mostly chill, but got super fun when me and Olivia went to Belmont Park, also known as the Mission Beach Boardwalk. We got there pretty late, but still had around 3 hours to ride the rollercoaster and spinny ride. On Sunday me and Olivia went to Pacific Beach. At first it was pretty cold and all cloudy, but we got lunch and the sun came out, so we were able to enjoy a couple hours of sunny beach time.
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