Water → HCID 22401687, compound

Participants

Reaction Steps

In 40 ml of dimethylformamide was dissolved 2.07 g (10.7 mmol) of Compound 1 prepared in Example 1, and 0.77 g (19.3 mmol) of sodium hydride (60%) and 2.56 ml (32.0 mmol) of ethyl iodide were added to the solution, followed by stirring at room temperature for 6 hours. After addition of water and evaporation of the solvent, the residue was subjected to partition between chloroform and water, and the chloroform layer was concentrated to dryness under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with chloroform-methanol (100:1). The first and second main fractions gave 1.24 g (53%) of Compound 26 and 0.51 g (22%) of Compound 27, respectively. Compound 26 and Compound 27 were recrystallized from dimethylformamide/water and ethanol, respectively, for purification.

Provenance & Evidence