反应详情

150 mg NaH are suspended in 20 ml tetrahydrofuran, and the mixture is cooled in ice. To this suspension is added a solution of 2.5 g ethyl 2-(4-bromo-3-(tetrahydropyran-2-yloxy)butanamido)acetate in 30 ml tetrahydrofuran. The mixture is stirred 40 min, then poured with stirring into a solution of 1 ml acetic acid in 10 ml water at 0° C. The solution is extracted with ether, the organic phase is washed with a saturated solution of NaHCO3, then washed with brine, dried and evaporated. The crude oil obtained is purified by chromatography on silica, eluting with ethyl acetate. A colourless oil is obtained, Rf 0.32 (silica gel plates, thickness 0.25 mm, eluent ethyl acetate).

1. temperaturethe mixture is cooled in ice
2. additionpoured
3. extractionThe solution is extracted with ether
4. washthe organic phase is washed with a saturated solution of NaHCO3
5. washwashed with brine
6. customdried
7. customevaporated
8. customThe crude oil obtained
9. customis purified by chromatography on silica
10. washeluting with ethyl acetate
11. customA colourless oil is obtained