反应详情

A solution of 4.02 g (0.01 mole) of crude (73%) 2-methyl-3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarbonyl chloride cis isomer in 20 ml of tetrahydrofuran was treated while stirring with 2 ml (0.02 mole) of 57% aqueous ammonium hydroxide. After stirring for 6 hr, the reaction mixture was diluted with 100 ml of water and the oil which separated was extracted into methylene chloride (2×50 ml). The combined extracts were dried over magnesium sulfate and concentrated in vacuo to give 4.2 g. A sample of the oil crystallized at -78° C. and was used to seed the bulk of the material. The resulting solid was recrystallized from benzene/isooctane to yield 2.35 g (87%) of white crystalline product, m.p. 107°-108° C.

1. additionwas treated
2. customthe oil which separated
3. extractionwas extracted into methylene chloride (2×50 ml)
4. dry with materialThe combined extracts were dried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customto give 4.2 g
7. customA sample of the oil crystallized at -78° C.
8. customThe resulting solid was recrystallized from benzene/isooctane