反应详情

温度

-78 °C

A mixture of 2.8 g (0.01 mole) of 3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarbonyl chloride and 1.4 g (0.01 mole) of potassium carbonate in 25 ml of tetrahydrofuran was stirred for 10 min then treated with 1.6 g (0.01 mole) of 4-phenylpiperidine. After stirring for 30 min, approximately 2 g of ice was added and stirring continued for 18 hr. The reaction mixture was diluted with 200 ml of water and the oil which separated was extracted into methylene chloride (2×50 ml). The extracts were combined, dried and concentrated in vacuo to yield 4.95 g of crude oil which solidified when cooled to -78° C. Recrystallization from isopropyl ether yielded 1.5 g (37%) of coarse white crystals, m.p. 72°-74° C.

1. stirringAfter stirring for 30 min
2. stirringstirring
3. waitcontinued for 18 hr
4. customthe oil which separated
5. extractionwas extracted into methylene chloride (2×50 ml)
6. customdried
7. concentrationconcentrated in vacuo
8. customto yield 4.95 g of crude oil which
9. customRecrystallization from isopropyl ether