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12th March 2013 @ 02:56

Repeat of AT-1-1 and AT-1-2 on a larger scale for synthesis of starting material, using MNR89-2 and recovered starting material from AT-1-1.

To MNR89 (5.28 g, 34.7 mmol, 1.0 equiv.) under argon was added POCl3 (53.2 g, 32.2 mL, 347 mmol, 10.0 equiv.) and the reaction mixture stirred at reflux for 4 h. The reaction mixture was cooled to rt and added to ice (approx. 400 mL) slowly. The mixture was stirred and solid sodium hydrogen carbonate was added slowly until effervescence ceased. The mixture was extracted into ethyl acetate (4 x 100 mL) and the combined organic phases dried (MgSO44) and concentrated under reduced pressure. The residue was purified by filtration through silica (4:1 hexanes:ethyl acetate) to give the product AT-1 (4.90 g, 83%) as a white solid. 

 

HIRAC

AT-1-3.pdf

 

NMR

AT-1-3.pdf

Attached Files
AT-1-3.pdf
AT-1-3.jpg
AT-1-3.pdf
osddAT-1-3.zip