反应详情

To a solution of 0.75 g (2.25 mmol) (4R,9aR)-6-(1-(R)-hydroxy-ethyl)-4-methyl-3,4,9,9a-tetrahydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester in 5 mL N,N-dimethylformamide 0.12 g (2.70 mmol) sodium hydride (55–65% dispersion in oil) was added. After 30 min., 0.28 mL (0.64 g, 4.50 mmol) methyl iodide was added and the reaction mixture was stirred at 50 deg C. for 2 h. After cooling down to room temperature, the reaction mixture was poured into 10% aqueous ammonium chloride solution and extracted three times with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate, filtered and evaporated. The residue was purified by column chromatography on silica gel (0.032–0.063 mm) with ethyl acetate:n-heptane (1:2) as eluant.

1. waitfor 2 h
2. extractionextracted three times with ethyl acetate
3. washThe combined organic layers were washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by column chromatography on silica gel (0.032–0.063 mm) with ethyl acetate:n-heptane (1:2) as eluant