反应详情

To a stirred solution of 90.0 mg (0.28 mmol) (4R,9aR)-7-hydroxy-4,6-dimethyl-3,4,9,9a-tetrahydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester (example 7, intermediate) in 1.0 mL N,N-dimethylformamide was added 14.8 mg (0.34 mmol) sodium hydride (55–65% dispersion in oil) and the reaction was stirred for 30 min. Then, 35 μl (80.0 mg, 0.56 mmol) methyl iodide was added. After 2 h the reaction mixture was diluted with ethyl acetate, washed with 10% aqueous sodium bicarbonate solution and brine, dried over magnesium sulfate and filtered. The solvent was removed at a rotary evaporator and the residue was purified by column chromatography on silica gel (0.032–0.063 mm) with ethyl acetate:n-hexane (1:1) as eluant.

1. washwashed with 10% aqueous sodium bicarbonate solution and brine
2. dry with materialdried over magnesium sulfate
3. filtrationfiltered
4. customThe solvent was removed at a rotary evaporator
5. customthe residue was purified by column chromatography on silica gel (0.032–0.063 mm) with ethyl acetate:n-hexane (1:1) as eluant