Water → HCID 22401676, compound

Participants

Reaction Steps

In 50 ml of dimethylformamide was dissolved 2.50 g (12.9 mmol) of Compound 1 prepared in Example 1, and 0.77 g (19.3 mmol) of sodium hydride (60%) and 2.20 ml (19.3 mmol) of butyl iodide were added to the solution, followed by stirring at room temperature for one hour. 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 2.30 g (71%) of Compound 32 and 0.84 g (26%) of Compound 33, respectively. Each compound was recrystallized from ethanol for purification.

Provenance & Evidence