Water → HCID 22401680, compound

Participants

Reaction Conditions

Reaction Steps

In 120 ml of dimethylformamide was dissolved 3.00 g (15.4 mmol) of Compound 1 prepared in Example 1, and 1.86 g (46.3 mmol) of sodium hydride (60%) and 7.48 ml (46.3 mmol) of tert-butyl bromoacetate were added to the solution, followed by stirring at 50° C. for 12 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 1.59 g (33%) of Compound 34 and 0.97 g (20%) of Compound 35, respectively. Each compound was recrystallized from ethanol for purification.

Provenance & Evidence