# Friday 8/2/2018¶

### Reduction of 2 to form 3 (AS08) Attempt 2¶

The reaction mixture had turned from deep blue to pale yellow and was reduced under vacuum to $$\sim$$10 mL and diluted with another $$\sim$$30 mL of DCM. The pH was checked at this point and determined to be $$\sim$$7.5, so not was added. The mixture was then washed with water (2$$\times$$40 mL) and $$\sim$$5.4 M brine (2$$\times$$40 mL). It was then dried with \$\ce{NaSO4}, filtered through celite and dried under vacuum, producing a yellow/white crude powder. The crude powder was redissolved in minimal DCM.

fig:AS08washing), an interesting solid formed in the interface between the organic and aqueous phases. I’m not entire sure what it could be, or if there’s anything in this reaction that could polymerise.

### Reduction of 2 to form 3 (AS05)¶

In playing around with this, I came up with a procedure that seems to work to precipitate out 3, however the precipitate is so fine (fig:AS05ppt2) that extracting it is proving difficult. I’ve come up with a plan (see Next week’s plan) to precipitate and extract this using the skillset I’ve learned in biochemistry, of precipitating, centrifuging and washing.

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Precipitated 3 from AS05

### Next week’s plan¶

1. Redissolve AS05 and AS08 in minimal DCM
2. Pipette AS05 and AS08 into microcentrifuge tubes
3. Dry the tubes till only 0.1 mL left
4. Add 1 mL of hexane:ethyl acetate (5:1)
5. Allow to precipitate
6. Centrifuge and pour off supernatant
7. Redissolve in 0.1 mL DCM in centrifuge tube
8. Add another 1 ml of hexane:ethyl acetate (5:1)
9. Allow to precipitate
10. Centrifuge and pour off supernatant
11. Pellet should now be pure 3