反应详情

温度

-70 °C

A mixture of 5.6 g (0.02 mole) of 1-chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine and 3 g (0.027 mole) of potassium carbonate in 50 ml of tetrahydrofuran was treated with 1.26 g (0.022 mole) of azetidine added dropwise to the stirred mixture. After stirring for 15 min, the reaction was treated with 10 g of ice and stirred for an additional 72 hr. The tetrahydrofuran was decanted from the salt-paste and concentrated on a rotary evaporator to yield an oil, 6.3 g. This oil crystallized when cooled to -70° C. and was recrystallized from hexane yielding 5.1 g (85%) of fine white crystals, m.p. 65°-68° C.

1. additionadded dropwise to the stirred mixture
2. stirringstirred for an additional 72 hr
3. customThe tetrahydrofuran was decanted from the salt-paste
4. concentrationconcentrated on a rotary evaporator
5. customto yield an oil, 6.3 g
6. customThis oil crystallized when
7. customwas recrystallized from hexane yielding 5.1 g (85%) of fine white crystals, m.p. 65°-68° C.