Hi, I am repeating the below procedures from a paper, but instead of adding the acid chloride dropwise in 30 minutes, I added the acid chloride in 4 separate intervals within 2 minutes. The reaction seemed to go well at first, but after around 4 hours I noticed some side products from TLC instead of the purple and red spot they described in the text.
Since the paper also did not mention how long the reaction took, I kept my reaction to stay reflux overnight. After 1 day, the TLC showed tailing trails on the "red spot" and some other minor side product spots. I kept go on to separate my product and obtained a brown material. The material is not my product, and I just wondered if it is so important to add the acid chloride dropwise? and how long should I let my reaction to react?
Thanks!!