反应详情

A sodium salt of p-cyanophenol(14.1 g) was dissolved in methyl ethyl ketone (20 ml), and chloromethyl 2-propynyl ether (Intermediate I-a) (10.6g, 0.1 mol) prepared in example 1 was added dropwise to the solution with stirring at room temperature. The reaction mixture was stirred for further 2 hours and the solvent was then evaporated off. The residue was extracted with toluene (30 ml) and the organic layer was washed with distilled water (20 g). The solvent was then evaporated off to obtain a crude reaction product (18.7 g). This was recrystallized from hexane (60 ml) to obtain 1-cyano-4-[(2-propynyloxy)methoxy]benzene (Intermediate II-i) (15.0 g, 79.7% yield). Its chemical purity by HPLC was 99.0%.

1. additionwas added dropwise to the solution
2. stirringThe reaction mixture was stirred for further 2 hours
3. customthe solvent was then evaporated off
4. extractionThe residue was extracted with toluene (30 ml)
5. washthe organic layer was washed with distilled water (20 g)
6. customThe solvent was then evaporated off
7. customto obtain a crude
8. customThis was recrystallized from hexane (60 ml)