反应详情

2.8 g (8.6 mmol) of 3-(4-benzyloxytetrahydrofuran-3-yloxy)-4-methoxybenzonitrile (A8) and 4.8 g (86.0 mmol) of potassium hydroxide are heated at 140° C. for 3 h in 30 ml of glycerol. The mixture is treated with 70 ml of water and acidified by dropwise addition of 40 ml of 2 N hydrochloric acid with ice-cooling. The mixture is subsequently stirred for 1 h, filtered and the precipitate is washed with ice water. For further purification, the product is chromatographed on silica gel [toluenelethyl acetate =2:1]. The product-containing fractions are concentrated and the residue is crystallized from isopropanol. 2.1 g of the title compound of m.p. 153-156° C. are obtained.

1. temperaturecooling
2. filtrationfiltered
3. washthe precipitate is washed with ice water
4. customFor further purification
5. customthe product is chromatographed on silica gel [toluenelethyl acetate =2:1]
6. concentrationThe product-containing fractions are concentrated
7. customthe residue is crystallized from isopropanol