5-(环丙基甲基)-2,2-二甲基-1,3-二恶烷-4,6-二酮

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of cyclopropanecarboxylic acid (17.2 g) in methylene chloride (800 mL) were added Meldrum's acid (28.8 g), WSCI.HCl (42.2 g) and 4-dimethylaminopyridine (39.1 g), and the mixture was stirred at room temperature for 18 hr. Water and then hydrochloric acid were added to acidify the reaction mixture, and the aqueous layer was removed by partitioning. Under ice-cooling, acetic acid (114 mL) and then sodium borohydride (18.9 g) were added slowly to the organic layer, and the mixture was stirred at room temperature for 3 days. Water and then hydrochloric acid were added to the reaction mixture, and the aqueous layer was removed by partitioning. The organic layer was concentrated to give a yellow powder. This was washed with ether/hexane to give the title compound (25.8 g) as a yellow powder. the aqueous layer was removed by partitioning Under ice-cooling acetic acid (114 mL) and then sodium borohydride (18.9 g) were added slowly to the organic layer the mixture was stirred at room temperature for 3 days Water and then hydrochloric acid were added to the reaction mixture the aqueous layer was removed by partitioning The organic layer was concentrated to give a yellow powder This was washed with ether/hexane