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1st October 2016 @ 22:22

Scheme:

Following [AEW 204-x]

 reaction scheme

Procedure:

The product of [rxn 1-2] (0.5397 g, 3.748 mmol, 1eq) was disolved in ethanol (20 mL). 4-(difluoromethoxy)benzaldehyde (0.482mL, 3.65 mmol, 0.97 eq) was added to the reaction mixture and the resulting solution was stirred under argon. A white precipitate quicly formed and 10 mL of ethanol was added to the reaction mixture. The reaction was allowed to stir overnight.

Workup (9-22):

The precipitate was recovered by vacuum filtration and washed with cold ethanol. An off-white powder (0.766 g, 2.91 mmol, 80%) was recovered. This crude product was not further purified.

NMR:

The product was disolved in CDCL3 and a 1H spectrum was recorded on a 500MHz instrument.

InChi:

InChI=1S/C4H5ClN4/c5-3-1-7-2-4(8-3)9-6/h1-2H,6H2,(H,8,9)

and

InChI=1S/C8H6F2O2/c9-8(10)12-7-3-1-6(5-11)2-4-7/h1-5,8H

to

InChI=1S/C12H9ClF2N4O/c13-10-6-16-7-11(18-10)19-17-5-8-1-3-9(4-2-8)20-12(14)15/h1-7,12H,(H,18,19)/b17-5+

Attached Files
step2completed.png
AMS_rxn2try2_PROTON_cdcl3_01.pdf
AMS_rxn2try2_PROTON_cdcl3_01.jcamp