反应详情

温度

100 °C

A mixture of (4S,7R)-2-(2,4-difluoro-phenyl)-7,8,8-trimethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (Intermediate 14; 200 mg, 0.65 mmol) and ethyl iodide (262 μL, 3.3 mmol) in dimethylformamide (2 mL) was heated at 100° C. over the weekend. The solvent was evaporated and ethyl acetate was added. The solution was washed twice with saturated aqueous sodium thiosulfate, and three times with water. The solution was dried (magnesium sulfate), filtered, evaporated, and purified by column chromatography, eluting with 75% ethyl acetate/petroleum ether, to give (4S,7R)-2-(2,4-difluoro-phenyl)-1-ethyl-7,8,8-trimethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (145 mg, 67%) as a white solid. IR 1667 cm−1.

1. customThe solvent was evaporated
2. additionethyl acetate was added
3. washThe solution was washed twice with saturated aqueous sodium thiosulfate, and three times with water
4. dry with materialThe solution was dried (magnesium sulfate)
5. filtrationfiltered
6. customevaporated
7. custompurified by column chromatography
8. washeluting with 75% ethyl acetate/petroleum ether