反应详情

To a solution of 0.65 g (2.0 mmol) (R)-6-chloro-4-methyl-3,4-dihydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester in 10 ml acetic acid was added 0.64 g (10.1 mmol) sodium cyano borohydride. After 3 h the reaction mixture was poured into 10% aqueous sodium carbonate solution and extracted twice with ethyl acetate. The organic layers were washed with brine, dried over magnesium sulfate, filtered and evaporated. The residue was purified by chromatography over silica gel (0.032–0.063 mm) with n-hexane:ethyl acetate (4:1) as eluant to afford the desired compound as a colorless oil (65.7%).

1. extractionextracted twice with ethyl acetate
2. washThe organic layers were washed with brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by chromatography over silica gel (0.032–0.063 mm) with n-hexane:ethyl acetate (4:1) as eluant