反应详情

A solution of (4R,7S)-2-(2,4-difluoro-phenyl)-7,8,8-trimethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (Intermediate 42; 153 mg, 0.5 mmol) and iodomethane (0.16 mL, 2.55 mmol) in N-methylpyrrolidine (1 mL) was heated at 100° C. in a sealed tube overnight. The reaction mixture was purified by preparative HPLC to give a brown semi-solid which was dissolved in ethyl acetate. The solution was washed with 10% aqueous sodium thiosulfate (three times) and brine, dried (sodium sulfate), filtered, and evaporated to give (4R,7S)-2-(2,4-difluoro-phenyl)-1,7,8,8-tetramethyl-1,2,4,5,6,7-hexahydro-4,7-methano-indazol-3-one (104 mg, 65%) as an off-white solid. ES(+)-MS (M+H) 319.

1. customThe reaction mixture was purified by preparative HPLC
2. customto give a brown semi-solid which
3. washThe solution was washed with 10% aqueous sodium thiosulfate (three times) and brine
4. dry with materialdried (sodium sulfate)
5. filtrationfiltered
6. customevaporated