Methyl iodide → HCID 90064493, compound

Participants

Reaction Conditions

Reaction Steps

To a reaction vessel, 10 g (0.025 mol) compound XIII and 100 ml tetrahydrofuran were added, stirred, under nitrogen, the mixture was cooled to −10-−15° C., 48 ml (0.096 mol, 2 mol/L) solution of lithium diisopropylamide in n-heptane was added dropwise for about 30 min, after the addition was complete, the reaction was kept for 30 min, and then 1.6 ml (0.026 mol) iodomethane was added dropwise, after the addition was complete, the mixture was warmed to room temperature and then stirred for 1 h, after the reaction was complete, 300 ml ethyl acetate and 150 ml water were added, extracted and washed, the organic layer was collected, dried over sodium sulfate, filtered, the filtrate was concentrated to dry under reduced pressure, separated by column chromatography, and 5.6 g compound XIV was obtained, with yield of 54.2%. MS (ESI): m/z 417 [M+H]+.

Provenance & Evidence