反应详情

A mixture, under argon, of 2.17 g of product from Example 113, 1.8 g of product from Example 28, 13.0 ml of N,N-diisopropyl ethylamine and 80 ml of acetonitrile is heated under reflux temperature for 8 hours. The reaction is cooled and concentrated in vacuo and dried under high vacuum for 1 hour. The crude residue is dissolved in 70 ml of tetrahydrofuran and 10.0 ml of 1M tetrabutyl ammonium fluoride in tetrahydrofuran is added and the mixture is stirred at room temperature, under argon, for 2.5 hours. The mixture is poured into water and extracted with ethyl acetate. The organic layer is washed with saturated sodium chloride, dried, filtered, and concentrated in vacuo to give 4.0 g of a brown oil. The oil is purified by chromatography (silica gel: 1%, 1.5% and 2% methyl alcohol/methylene chloride)to give 2.1 g of the desired product.

1. temperatureunder reflux temperature for 8 hours
2. temperatureThe reaction is cooled
3. concentrationconcentrated in vacuo
4. customdried under high vacuum for 1 hour
5. dissolutionThe crude residue is dissolved in 70 ml of tetrahydrofuran
6. addition10.0 ml of 1M tetrabutyl ammonium fluoride in tetrahydrofuran is added
7. additionThe mixture is poured into water
8. extractionextracted with ethyl acetate
9. washThe organic layer is washed with saturated sodium chloride
10. customdried
11. filtrationfiltered
12. concentrationconcentrated in vacuo