Diethyl Ether → HCID 67958972, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 2-methyl-pyrimidine-5-carbaldehyde oxime (145 gm) in DMF (435 ml) was added N-chlorosuccinamide (169.6 gm) in portions at 30° C. for 0.5 h. As the TLC indicated completion of the reaction, diethyl ether (1450 ml) was added. The reaction mixture was cooled to −5° to 0° C. To a cooled reaction mixture, was added triethylamine (589 ml) followed by trimethylsilylacetylene (450 ml). The mixture was stirred at −5° C. for additional 1 h. The solid separated was filtered at suction. Filtrate was washed with water (300 ml×4) followed by brine solution (500 ml) and organic layer was concentrated under vacuum to provide a solid in 158 gm quantity which was used as it is for further reaction.

Provenance & Evidence