Hydrochloric Acid → N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydrophthalimide

温度

80 °C

Cyclopentyl p-toluenesulfonate (1.90 g, 8.11 mmol) was added to a solution of N-(2-fluoro-4-chloro-5-hydroxyphenyl)-3,4,5,6-tetrahydrophthalimide (2.0 g, 6.76 mmol) and potassium carbonate (0.60 g, 4.34 mmol) in acetonitrile (50 ml), followed by stirring for 2 hours at 80° C. After completion of the reaction, 1N hydrochloric acid (20 ml) was added to the resulting reaction mixture, and the mixture was extracted with ethyl acetate (20 ml×3 times). The organic layer was washed with water, dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Ethanol (5 ml) was added to the resulting pale yellow oily substance, and the precipitated N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydrophthalimide as a white solid (0.77 g 2.12 mmol, 31.4% yield) was isolated by filtration. The spectral data and the like are as described in Example 1.

1. additionwas added to the resulting reaction mixture
2. extractionthe mixture was extracted with ethyl acetate (20 ml×3 times)
3. washThe organic layer was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. additionEthanol (5 ml) was added to the resulting pale yellow oily substance

ORDレコード

ord-c1837d730b9a491eb819c9ec4ff215ce

出典データセット

uspto-grants-1995_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05464811