反应详情

温度

90 °C

Caesium carbonate (39.4 g) was added to a solution of 4-hydroxymethyl-phenol (10 g) and 2-bromo-1,1-diethoxyethane (12.73 mL) in DMF (200 mL) and the resulting mixture stirred at 90° C. for 16 h. The reaction was poured into water (500 mL) and extracted with ethyl acetate (3×250 mL). The combined organic solutions were washed with water (250 mL) and brine (250 mL), then dried over sodium sulphate, filtered and evaporated in vacuo. Purification was by silica gel chromatography eluting with an isohexane to diethyl ether gradient to give the subtitled compound as a yellow oil. Yield 9.5 g.

1. extractionextracted with ethyl acetate (3×250 mL)
2. washThe combined organic solutions were washed with water (250 mL) and brine (250 mL)
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. customevaporated in vacuo
6. customPurification
7. washeluting with an isohexane to diethyl ether gradient