Potassium Iodide → HCID 10665070, compound

Participants

Reaction Conditions

Reaction Steps

2 g of anhydrous potassium carbonate are added, under an inert atmosphere, to a solution of 2 g of the product of Step A in 50 ml of anhydrous dimethylformamide. After stirring for 15 minutes at 65° C., 2.4 g of anhydrous potassium iodide and 4.4 g of 3-chloro-3-methyl-1-butyne are added and the reaction mixture is maintained at 65° C. for 24 hours and then at 130° C. for 1 hour 30 minutes. After cooling, the solution is hydrolysed and then extracted with dichloromethane. The combined organic phases are washed with water and then with a 1M potassium hydroxide solution, dried over sodium sulphate and then evaporated. Chromatography over silica gel (cyclohexane/acetone: 90/10) yields 1.10 g of the expected product.

Provenance & Evidence