反应详情

温度

100 °C

3-(bromomethyl)-3-(methoxymethyl)oxetane (0.35 g, 0.18 mmol) preparation described in example 24) and 6-bromo-2,3-dimethoxyphenol (0.21 g, 0.9 mmol) (preparation described in Preparation 1) were dissolved in DMF (8 mL). K2CO3 (0.31 g, 2.2 mmol) was added. The suspension was heated in a microwave oven at 100° C. for 10 min. H2O was added and the mixture was extracted with EtOAc (×2). The combined organic phases were washed with brine, dried (Na2SO4), filtered and concentrated. Purification by flash chromatography (Heptane:EtOAc 100:0->75:25) yielded 3-(6-Bromo-2,3-dimethoxy-phenoxymethyl)-3-methoxymethyl-oxetane as an oil.

1. extractionthe mixture was extracted with EtOAc (×2)
2. washThe combined organic phases were washed with brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification by flash chromatography (Heptane:EtOAc 100:0->75:25)