反应详情

To a solution of ethyl 4-(3-(2-tert-butylphenoxy)azetidin-1-yl)-4-oxobutanoate (0.47 g, 1.41 mmol) obtained in Example 11 in ethanol (20.0 mL) was added lithium hydroxide (1.0M aqueous solution, 4.23 ml, 4.23 mmol) under ice-cooling, and the mixture was stirred at room temperature. After 2 hr, the reaction mixture was adjusted to about pH 1 with 1.0M hydrochloric acid, and the mixture was concentrated under reduced pressure. The obtained residue was partitioned to between ethyl acetate and water, and the organic layer was washed with saturated sodium chloride, dried (Na2SO4), filtered, and concentrated under reduced pressure. The residue was recrystallized from heptane/ethyl acetate to give the title compound (0.28 g, 65%) as a white powder.

1. temperaturecooling
2. concentrationthe mixture was concentrated under reduced pressure
3. customThe obtained residue was partitioned to between ethyl acetate and water
4. washthe organic layer was washed with saturated sodium chloride
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was recrystallized from heptane/ethyl acetate