反应详情

To 10 ml of diethylamine was added with stirring 0.5 g (5.1 mmol) of 4-pentynoic acid, 1.4 g (5 mmol) of 1-bromo-2-iodobenzene, and 60 mg (0.05 mmol) of tetrakis(triphenylphosphine)palladium(0) The slurry was degassed with argon and 0.19 g (1.0 mmol) of CuI was added. The reaction mixture was stirred for 2 hr. at room temperature and then poured into approximately 100 ml of a 10% HCl solution. The resulting precipitate was filtered, washed with water and dried. The solid was taken up in hot CHCl3 and filtered to remove insoluble salts. After evaporation of the solvent, the resulting orange solid was recrystallized from a a chloroform-hexane mixture to produce a tan solid, m.p. 87°-91° C.

1. additionwas added
2. filtrationThe resulting precipitate was filtered
3. washwashed with water
4. customdried
5. filtrationfiltered
6. customto remove insoluble salts
7. customAfter evaporation of the solvent
8. customthe resulting orange solid was recrystallized from a a chloroform-hexane mixture
9. customto produce a tan solid, m.p. 87°-91° C.