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28th January 2014 @ 22:28
Reaction proceeded as expected. Product was obtained in 87% yield. START: 28/01/14 FINISH: 31/01/14 [b][u]Scheme[/u][/b] [b][u]Hazard and Risk Assessment[/u][/b] [data]5317[/data] [b][u]Procedure[/u][/b] [b]28/01/14.[/b] Suspended KAB8-17 in ethanol and HCl (1 M). Heated to reflux from 1500; oil bath approx. 130 ° C. Yellowish heterogenous solution. [b]29/01/14.[/b] 0800, clear mixture homogenous and orange. Allowed to cool. Basified to pH 11-13 using solid KOH (about 4 g). Extracted with dichloromethane (2 × 100 mL) and ethyl acetate (100 mL). Combined organic fractions were dried with Na2SO4, concetrated under reduced pressure and dried in vacuo to give an orange solid (1.49 g, 87%) HNMR consistent with the expected product. No purification required. [data]5319[/data][data]5317[/data] --------------------------------------------
Attached Files
Scheme KAB119-1
HNMR KAB119-1 300 MHz CDCl3
Raw HNMR KAB119-1 300 MHz CDCl3
HIRAC KAB119-1