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 1.6 g (0.02 mole) of 40% aqueous monomethylamine. 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 (4.2 g). The oil solidified on standing and was recrystallized from isooctane with a trace of benzene to give 2.6 g (90.3%) of white crystalline product, m.p. 89°-91° 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 (4.2 g)
6. customwas recrystallized from isooctane with a trace of benzene