反应详情

A mixture, under argon, of 2.0 g of product from Example 114, 15 ml of 1N sodium hydroxide, 5.4 ml of 2-chloroethyl-p-toluene sulfonate and 70 ml of 2-butanone is heated at reflux temperature for 18 hours. The mixture is cooled, concentrated in vacuo and the residue partitioned between ethyl acetate and water. The organic layer is washed with saturated sodium chloride, dried, and concentrated in Vacuo to give an oil. The oil is purified by chromatography (silica gel: methylene chloride, 0.5%, 1.0% and 1.5% methyl alcohol/methylene chloride) to give 1.7 g of the desired product.

1. temperatureat reflux temperature for 18 hours
2. temperatureThe mixture is cooled
3. concentrationconcentrated in vacuo
4. customthe residue partitioned between ethyl acetate and water
5. washThe organic layer is washed with saturated sodium chloride
6. customdried
7. concentrationconcentrated in Vacuo
8. customto give an oil
9. customThe oil is purified by chromatography (silica gel: methylene chloride, 0.5%, 1.0% and 1.5% methyl alcohol/methylene chloride)