Water → HCID 69331493, compound

Participants

Reaction Conditions

Reaction Steps

0.12 g (5.12 mmol, 50%) of sodium hydride was added to a solution of 2.25 g (5.11 mmol) of the compound from example 12b in 40 ml of dry DMF at 0° C. and stirred at this temperature for 5 min. The mixture was then allowed to reach RT, was stirred for 1 h, was again cooled to 0° C. and then 1.47 g (5.11 mmol) of the compound from example 1b were added in one portion. Stirring was continued at this temperature for 30 min, then 50 ml of water were added while cooling in ice, and the mixture was extracted three times with CH2Cl2. The combined organic phases were dried over Na2SO4, filtered and concentrated. The residue was purified by chromatography on silica gel. 3.15 g of the title compound were obtained.

Provenance & Evidence