反应详情

1 -Cyano-4-[(2-propynyloxy)methoxy]benzene (Intermediate II-i) (9.4 g, 0.05 mol) prepared in the above example 4 and 48% w/v aqueous sodium hydroxide solution (11.3 g) were added to methanol (75 g). Iodine (14.0 g, 0.055 mol) was then added to the solution in several portions while maintaining the inner temperature below 10° C. The reaction mixture was stirred for further 3 hours and the solvent was then evaporated off. The residue was extracted with toluene (10 ml) and the toluene layer was washed with distilled water. Toluene was then evaporated off to obtain a crude reaction product (15.3 g). The crude reaction product (15.3 g) was recrystallized from hexane (50 ml) to obtain the desired 1-cyano-4-[[(3-iodo-2-propynyl)oxy]methoxy]benzene (Derivative III-i)(12.6 g, 94% yield).

1. temperaturewhile maintaining the inner temperature below 10° C
2. customthe solvent was then evaporated off
3. extractionThe residue was extracted with toluene (10 ml)
4. washthe toluene layer was washed with distilled water
5. customToluene was then evaporated off
6. customto obtain a crude
7. customwas recrystallized from hexane (50 ml)