反应详情

温度

100 °C

A mixture of (4S,7R)-2-(2-chloro-4-fluoro-phenyl)-7,8,8-trimethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (Intermediate 21; 290 mg, 0.90 mmol) and iodomethane (0.15 mL, 2.3 mmol) in N,N-dimethylformamide (5 mL) was heated at 100° C. overnight. Water was added and the reaction mixture was extracted three times with ethyl acetate. The combined organic extracts were washed with water and brine, dried (magnesium sulfate), filtered, and evaporated to give (4S,7R)-2-(2-chloro-4-fluoro-phenyl)-1,7,8,8-tetramethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (260 mg, 86%) as a yellow solid. ES(+)-MS (M+H) 335.

1. extractionthe reaction mixture was extracted three times with ethyl acetate
2. washThe combined organic extracts were washed with water and brine
3. dry with materialdried (magnesium sulfate)
4. filtrationfiltered
5. customevaporated