反应详情

温度

0 °C

A solution of {2-[(tetrahydro-2H-pyran-2-yloxy)methyl]phenyl}methanol (5.52 g, 24.84 mmol) in CH2Cl2 (100 ml) was cooled to 0° C. and treated with Et3N (6.92 ml, 49.68 mmol) followed by the addition of Ts2O (8.9 g, 27.33 mmol). The reaction stirred at 0° C. for 3.5 hours. The mixture was diluted with sat. NH4Cl and extracted with CH2Cl12 (2×). The combined organic solutions were washed with water, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by normal phase chromatography (10% EtOAc/hexanes—20%) to give a light brown oil (7.36 g).

1. extractionextracted with CH2Cl12 (2×)
2. washThe combined organic solutions were washed with water
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by normal phase chromatography (10% EtOAc/hexanes—20%)