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 was added 0.12 g (2.70 mmol) sodium hydride (55–65% dispersion in oil). 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 to room temperature the reaction mixture, was poured onto 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 chromatographed 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 chromatographed on silica gel (0.032–0.063 mm) with ethyl acetate:n-heptane (1:2) as eluant