Potassium Carbonate → HCID 50905028, compound

Participants

Reaction Steps

Hydrogenation: the crude melted product was charged to an autoclave and diluted with 100 mL of isopropyl alcohol. 1.55 g of 5% Pd/C were added, and after flushing with nitrogen, the hydrogenation was carried out at 65° C. and 6 bar of H2 for 6 hrs. The mixture was cooled to room temperature and filtered on a celite pad to remove the catalyst. The organic solution was evaporated u.v. (20° C./21 mbar) and the residue distilled at 104°-112° C./0.1 mbar. 61 g of 5-hydroxy-6-propyl benzo[1.3]dioxole were obtained. Following the same procedure as in Example 3 c), 61 g. of 5-hydroxy-6-propyl benzo[1.3]dioxole were reacted with 45.9 g (0.34 moles) of 1-bromo-2-butyne and 47.7 g (0.34 moles) of anhydrous potassium carbonate in 250 ml of acetone. The filtrate in evaporated u.v. (20° C./ 21 mbar) and 69.1 g of 5-(but-2-ynyloxy)-6-propyl-benzo[1.3]dioxole were obtained (purity 75.5%).

Provenance & Evidence