Water → HCID 13491594, compound

Participants

Reaction Steps

20 g (0.524 mol) of LiAlH4 are suspended in 400 ml of absolute diethyl ether at room temperature, with stirring, while flushing with nitrogen and in the absence of moisture. 550 ml of absolute tetrahydrofuran are then added, followed by 34 g (0.116 mol) of 8-methyl-6-phenyl-6,7,8,9-tetrahydro-1H-pyrido[4,3-g]indole-2,3-dione in portions. The reaction mixture is subsequently stirred at room temperature for 31/2 hours. To dissociate the reaction complex, a solution of 42 ml of H2O in 160 ml of tetrahydrofuran is added dropwise, with cooling. The inorganic solid is filtered off and the filtrate is freed from the solvent on a rotary evaporator. The residue is chromatographed on silica gel 60 with an eluent mixture of: ethyl acetate and 8.3% of MeOH. The pure substance is dried in a desiccator over P2O5 at 60° C. under a water pump vacuum.

Provenance & Evidence