Sodium hydride → HCID 11657009, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of the title compound from Example 261 (1.0 grams) in dry DMF (60 mL) was added HOBT (1.4 grams), sodium hydride (0.2 grams, 60% in mineral oil) and distilled water (0.5 mL). The solution was stirred at 25° C. under nitrogen while being irradiated with a 200 Watt lamp for 20 hours. The reaction mixture was concentrated in vacuo, diluted with CH2Cl2 and saturated aqueous sodium bicarbonate and after two hours, the organic phase was separated, dried over MgSO4 and concentrated. Purification by flash column chromatography (silica gel) using 3-5% MeOH--CH2Cl2 afforded the title compound (Yield 1.1 grams, 87%, MH+564).

Provenance & Evidence