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14th February 2014 @ 05:08

Github Tag: Issue #155

Procedure:

AEW 116-1 (100 mg, 0.27 mmol, 1 equiv.) was dissolved in EtOH (1 mL) and then hydrazine hydrate (0.135 mL, 2.7 mmol, 10 equiv.) was added and the mixture stirred at 80 ˚C for 20 h (12 h sufficient for other reactions but just left longer as I came in later on Saturday). The reaction mixture was evaporated at the toxic buchi to give a yellow/orange solid. NMR seemed to show possible by-products and the mixture wasn't completely soluble in CDCl3 so decided to work up.

Reaction mixture was dissolved in EtOAc, washed with a saturated aqueous solution of NaHCO3 and then water, brine, dried (MgSO4), filtered and evaporated to give an orange soild that looked better by 1H NMR and was used as crude in the next reaction.

Data:

AEW 118-1 crude.zip
AEW 118-1 work up.zip

Hazard and Risk Assessment:

HIRAC AEW 118-1.pdf

InChi String:

InChI=1S/C13H6ClF6N3O/c14-10-5-21-4-9(23-10)11(24)22-8-2-6(12(15,16)17)1-7(3-8)13(18,19)20/h1-5H,(H,22,24)

to

InChI=1S/C13H9F6N5O/c14-12(15,16)6-1-7(13(17,18)19)3-8(2-6)22-11(25)9-4-21-5-10(23-9)24-20/h1-5H,20H2,(H,22,25)(H,23,24)

Attached Files
AEW 118-1.cdxml
AEW 118-1.png
HIRAC AEW 118-1.pdf
AEW 118-1 crude.zip
AEW 118-1 work up.zip