反应详情

To a stirred mixture of 30.4 parts of 1,3-propanediol and 90 parts of N,N-dimethylformamide were added 5.28 parts of a sodium hydride dispersion 50% at a temperature below 20° C. Stirring was continued for 2 hours at room temperature under nitrogen atmosphere. Then there were added dropwise 15.9 parts of 1,4-difluoro-2-nitrobenzene so that the temperature had been maintained below 30° C. Upon completion, stirring was continued overnight at room temperature. The reaction mixture was poured onto water and the product was extracted with trichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the eluent was evaporated, yielding 21.5 parts 3-(4-fluoro-2-nitrophenoxy)propanol as a residue (intermediate 24).

1. temperaturehad been maintained below 30° C
2. stirringUpon completion, stirring
3. waitwas continued overnight at room temperature
4. additionThe reaction mixture was poured onto water
5. extractionthe product was extracted with trichloromethane
6. washThe extract was washed with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. customThe residue was purified by column-chromatography over silica gel
11. customThe pure fractions were collected
12. customthe eluent was evaporated