反应详情

温度

140 °C

(±) 1-Azabicyclo[2.2.2]octane-3-carboxylic acid hydrazide (D8) (0.36 g; 2.1 mmoles) and triethyl orthoacetate (3 ml) were heated at 120° C. for 2 h. Excess triethyl orthoacetate was evaporated in vacuo and the residue was heated for a further 2 h at 140° C. The reaction was diluted with water (10 ml), saturated with potassium carbonate and extracted into ether (3×15 ml). Combined organic extracts were dried (Na2SO4) and concentrated to give the title compound as an oil (0.29 g; 72%), which was purified as the oxalate salt. m.p. 147°-8° (Acetone-methanol).

1. customExcess triethyl orthoacetate was evaporated in vacuo
2. additionThe reaction was diluted with water (10 ml), saturated with potassium carbonate
3. extractionextracted into ether (3×15 ml)
4. dry with materialCombined organic extracts were dried (Na2SO4)
5. concentrationconcentrated