反应详情

At below 5° C., 5.0 g of 2-(2-bromoethyl)-3-bromomethylthiophene obtained in Example 7 was dissolved in 50 mL of acetonitrile, and added thereto was a solution obtained by dissolving 2.7 g of 2-chlorobenzylamine and 6.8 g of diisopropylethylamine in 25 mL of acetonitrile. The resulting mixture was refluxed for 5 hours, and concentrated by evaporation under reduced pressure. The residue was dissolved in 100 mL of ethyl acetate, and washed twice with 70 mL portions of water. The organic layer was washed with 50 mL of saturated sodium chloride aqueous solution and concentrated under reduced pressure. The dark yellow colored oily residue thus obtained was subjected to a silica gel column chromatography (eluent, n-hexane:ethyl acetate=5:1) to obtain 3.6 g (yield of 78%) of the title compound as a yellowish oil.

1. additionadded
2. customobtained
3. temperatureThe resulting mixture was refluxed for 5 hours
4. concentrationconcentrated by evaporation under reduced pressure
5. dissolutionThe residue was dissolved in 100 mL of ethyl acetate
6. washwashed twice with 70 mL portions of water
7. washThe organic layer was washed with 50 mL of saturated sodium chloride aqueous solution
8. concentrationconcentrated under reduced pressure
9. customThe dark yellow colored oily residue thus obtained