反应详情

Sodium hydride (content: 62%; 60 mg) was gradually added to anhydrous ethanol (10 ml) and dissolved. A solution of the ester (314 mg; prepared in reference example 26) in anhydrous ethanol (1 ml) was added to the solution. The mixture was stirred for 4 hr. at 70° C. and then for 30 min at 80° C. Glacial acetic acid (210 mg) was added to the reaction solution with ice-cooling to stop the reaction. The solvent was removed from the reaction solution under reduced pressure. The residue was diluted with ether. The mixture was washed with water. Aqueous layer was removed. Ethereal layer was dried over anhydrous magnesium sulfate and then evaporated. The residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=2:1) to give the title compound (122 mg) having the following physical data.

1. dissolutiondissolved
2. waitat 70° C. and then for 30 min at 80° C
3. temperaturecooling
4. customthe reaction
5. customThe solvent was removed from the reaction solution under reduced pressure
6. additionThe residue was diluted with ether
7. washThe mixture was washed with water
8. customAqueous layer was removed
9. dry with materialEthereal layer was dried over anhydrous magnesium sulfate
10. customevaporated
11. customThe residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=2:1)