反应详情

A mixture of 5.04 g (40 mmol) 3-fluorobenzyl alcohol and 1.29 g (4 mmol) tris-(dioxa-3,6-heptyl)amine is treated with 2.47 g (44 mmol) of potassium hydroxide. The mixture is stirred at room temperature for 10 min, then 5.55 g (44 mmol) of 4-fluoro-nitrobenzene is slowly added through a dropping funnel. The mixture is kept for 45 min at 80° C., cooled to room temperature and diluted with about 75 ml water. Extraction with ethyl acetate and washing with 2M aqueous hydrochloric acid yields a yellowish organic phase, which is dried and evaporated. The residue is recrystallised from methanol to give 6.07 g (61%) of the title compound. Yellow crystals, mp=104-105° C.

1. waitThe mixture is kept for 45 min at 80° C.
2. temperaturecooled to room temperature
3. extractionExtraction with ethyl acetate
4. washwashing with 2M aqueous hydrochloric acid
5. customyields a yellowish organic phase, which
6. customis dried
7. customevaporated
8. customThe residue is recrystallised from methanol