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8th October 2016 @ 03:24

Scheme:

Following [AEW 204-x]

 reaction scheme

Procedure:

A sample of the Reaction 1 product, 2-Chloro-6-hydrazinylpyrazine (1.17g, 8.125mmol, 1eq) was dissolved in ethanol (35 mL, 95% v/v). 4-(difluoromethoxy)benzaldehyde (1.1 mL, 8.125mmol, 1eq) was added to the reaction mixture and the resulting solution was stirred under argon. A white precipitate formed and 20 mL of ethanol was added to the reaction mixture. The reaction was allowed to stir for 72 hours.

Workup (10-2-16)


The precipitate was recovered by vacuum filtration and washed with cold ethanol (30 mL, 95% v/v) and was connected to the high vacuum for 1 hour. A yellow-white powder (1.68 g, 6.38mmol, 79%) was recovered. This crude product was not further purified.

 

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
CNMR_rxn2r4_dmso_CARBON_dmso_01.pdf
CNMR_rxn2r4_dmso_CARBON_dmso_01.jcamp
HNMR_rxn2r4_dmso_PROTON_dmso_01.pdf
HNMR_rxn2r4_dmso_PROTON_dmso_assign.jcamp
TLC Reaction 2-4 Annotated.jpg
Step 2 r4 picture 10-2-16.jpg
TLC rxn 2 master.jpg
Reaction 2-4 GCMS.pdf