Tuesday 12/2/2018¶

Reduction of 2 to form 3 (AS08) Attempt 2 and (AS05)¶

Each sample was redissolved in minimal DCM and transferred to a microcentrifuge tube. From here the samples were reduced with warm airflow until they were both $$\sim$$0.1 mL in volume. The the microcentrifuge tubes was added $$\sim$$1 mL of hexane:ethyl acetate (5:1) and was allowed to precipitate.

Out of AS05 fell a dark brown precipitate and out of AS08 fell a small amount of white precipitate. I wasn’t happy with how much fell out of solution, so I reduced the samples again with hot airflow, to try with a higher proportion of hexane:ethyl acetate.