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Reaction proceeded as expected. Product was obtained in 87% yield.
START: 28/01/14
FINISH: 31/01/14
Scheme
Hazard and Risk Assessment
Procedure
28/01/14. Suspended KAB8-17 in ethanol and HCl (1 M). Heated to reflux from 1500; oil bath approx. 130 ° C. Yellowish heterogenous solution.
29/01/14. 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.
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START: 28/01/14
FINISH: 31/01/14
Scheme
Hazard and Risk Assessment
Procedure
28/01/14. Suspended KAB8-17 in ethanol and HCl (1 M). Heated to reflux from 1500; oil bath approx. 130 ° C. Yellowish heterogenous solution.
29/01/14. 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.
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