反应详情

A solution of the product from Step A (2.88 g, 8.86 mmol) in acetone (100 mL) was degassed with reduced pressure and nitrogen. Powdered potassium carbonate (1.35 g, 9.75 mmol) and propargyl bromide (80% by weight in toluene, 0.99 mL, 8.86 mmol) were added the mixture was refluxed for 24 hours. The cooled reaction mixture was filtered and the filtrate was evaporated to a yellow oil (3.15 g) which was purified by chromatography (silica, 20% to 50% ethyl acetate in hexane) to give a white solid (2.37 g, 74%): mp 104-106° C.; LC/MS (+APCI) m/z 364 (M+H).

1. temperaturewas refluxed for 24 hours
2. customThe cooled reaction mixture
3. filtrationwas filtered
4. customthe filtrate was evaporated to a yellow oil (3.15 g) which
5. customwas purified by chromatography (silica, 20% to 50% ethyl acetate in hexane)