反应详情

Lithium aluminium hydride (792 mg, 19.8 mmol) was suspended in THF (6 ml) and cooled in an ice bath. A solution of 4,7-difluoro-isobenzofuran-1,3-dione (730 mg, 3.97 mmol) in THF (6 ml) was added during 5 min. After completion of the reaction (5 min), diethyl ether (30 ml) was added. Subsequently, 2 ml of EA were added in order to decompose excess of lithium aluminium hydride, and thereafter water was slowly added until the alumina salts precipitated. The supernatant was decanted and the precipitate washed twice with EA. The combined extracts were dried over sodium sulfate, filtered and evaporated to dryness to yield 360 mg of the title compound.

1. temperaturecooled in an ice bath
2. additionwas added
3. customprecipitated
4. customThe supernatant was decanted
5. washthe precipitate washed twice with EA
6. dry with materialThe combined extracts were dried over sodium sulfate
7. filtrationfiltered
8. customevaporated to dryness