Dimethylformamide → HCID 9795316, compound

Participants

Reaction Steps

0.57 g 2-fluoronitrobenzene, 0.65 g morpholino-propanol, 3.0 g caesium carbonate and 30 ml dimethylformamide are stirred for 2 days at room temperature in a closed 50 ml round-bottomed flask. One pours the suspension on to 50 ml water, extracts the aqueous phase 3 times with, in each case, 50 ml ethyl acetate and evaporates the combined organic phases on a rotoevaporator. For the removal of the dimethylformamide, which would disturb the chromatographic separation, the DMF-containing residue is again evaporated 2 to 3 times, together with some toluene, at 50° C. and 30 mbar vacuum. The oily residue is then purified on silica gel (0.04 to 0.063 mm) at 0.1 bar by flash chromatography. Once obtains 0.9 g of oil (82.4%).

Provenance & Evidence