反应详情

温度

75 °C

To a solution of ({[(2R)-2-(2,2-diethoxyethoxyl)hex-4-en-1-yl]oxy}methyl)benzene (C13) (350 g from the previous step, ≦0.64 mol) in tetrahydrofuran (1.4 L) was added aqueous hydrochloric acid (2 M, 700 mL), and the reaction mixture was stirred at 75° C. for 1 hour. Solvent was removed in vacuo and the aqueous residue was extracted with ethyl acetate (2.0 L). The combined organic layers were washed with saturated aqueous sodium chloride solution (3×500 mL), dried over sodium sulfate, filtered, and concentrated under reduced pressure. The product was obtained as a pale brown oil (210 g, ≦0.64 mol), which was taken directly to the following step.

1. customSolvent was removed in vacuo
2. extractionthe aqueous residue was extracted with ethyl acetate (2.0 L)
3. washThe combined organic layers were washed with saturated aqueous sodium chloride solution (3×500 mL)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure