反应详情

A mixture of 2.8 g (0.01 mole) of 3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarbonyl chloride and 4.2 g (0.03 mole) of potassium carbonate in 25 ml of tetrahydrofuran was stirred for 10 min, then treated with 2.9 g (0.01 mole) of 1-propylpiperazine dihydrobromide in small portions. After 30 min, a few pieces of ice were added. After stirring for 17 hr, the reaction was diluted with 200 ml of water then extracted with methylene chloride (2×50 ml). The combined extracts were dried over magnesium sulfate and concentrated in vacuo, yielding 4.84 g of crude residue. The residue was converted to the fumarate salt in 2-propanol, concentrated to a solid in vacuo and recrystallized from acetone with a trace of ethanol to yield 2.9 g (59.5%) of fine white crystals; m.p. 117°-123° C.

1. waitAfter 30 min
2. additiona few pieces of ice were added
3. stirringAfter stirring for 17 hr
4. extractionthen extracted with methylene chloride (2×50 ml)
5. dry with materialThe combined extracts were dried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customyielding 4.84 g of crude residue
8. concentrationconcentrated to a solid in vacuo
9. customrecrystallized from acetone with a trace of ethanol