反应详情

Twenty-one parts of 2-(4-chloro-2-fluorophenyl)-2,-3,4,5,6,7-hexahydro-3-hydroxy-3-methyl-1H-isoindol-1-one and one part of potassium bisulfate were heated with occasional stirring in an oil bath at 160°-170° for 15 minutes. The melt was poured into 200 parts of chloroform and washed successively with 100 parts of water, 50 parts of 10% aqueous sodium hydroxide and 100 parts of saturated aqueous sodium chloride solution. After drying the organic phase with anhydrous sodium sulfate, the solvent was evaporated at 300 mm. Hg at 50°. The residue was crystallized from 100 parts of absolute ethanol to yield 10.1 parts of 2-(4-chloro-2-fluorophenyl)-2,3,4,5,6,7-hexahydro-3-methylene-1H-isoindol-1-one melting at 84.0°-85.5°.

1. washwashed successively with 100 parts of water, 50 parts of 10% aqueous sodium hydroxide and 100 parts of saturated aqueous sodium chloride solution
2. dry with materialAfter drying the organic phase with anhydrous sodium sulfate
3. customthe solvent was evaporated at 300 mm. Hg at 50°
4. customThe residue was crystallized from 100 parts of absolute ethanol