反应详情

温度

40 °C

A mixture of 400 mg of the hydroxymethyl compound (prepared as described in Reference Example 4), 5 ml of benzene and 196 μl of thionyl chloride was stirred at 40° C. for one hour, and concentrated under reduced pressure. To the residue was added a saturated aqueous solution of sodium bicarbonate, and the mixture extracted with chloroform. The extract was washed with water, dried over magnesium sulphate and concentrated under reduced pressure. To the residue was added 5 ml of acetic acid and 175 mg of zinc powder, and the mixture stirred at room temperature for one hour, and then concentrated under reduced pressure. To the residue was added a saturated aqueous solution of sodium bicarbonate, and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulphate and concentrated under reduced pressure to give 166 mg of the title compound having the following physical characteristics:

1. concentrationconcentrated under reduced pressure
2. additionTo the residue was added a saturated aqueous solution of sodium bicarbonate
3. extractionthe mixture extracted with chloroform
4. washThe extract was washed with water
5. dry with materialdried over magnesium sulphate
6. concentrationconcentrated under reduced pressure
7. additionTo the residue was added 5 ml of acetic acid and 175 mg of zinc powder
8. stirringthe mixture stirred at room temperature for one hour
9. concentrationconcentrated under reduced pressure
10. additionTo the residue was added a saturated aqueous solution of sodium bicarbonate
11. extractionextracted with ethyl acetate
12. washThe extract was washed with water
13. dry with materialdried over magnesium sulphate
14. concentrationconcentrated under reduced pressure