Water → HCID 21277439, compound

Participants

Reaction Steps

1 ml of acetyl chloride in 5 ml of absolute tetrahydrofuran was added dropwise, at 20° C., to a solution of 3 g (8 millimoles) of the benzylamine derivative from Example 30, 1.6 g (16 millimoles) of triethylamine and 50 mg of DMAP (4-N,N-dimethylaminopyridine) in 25 ml of absolute tetrahydrofuran. After 1 hour at 0° C., the mixture was poured onto 100 ml of water and extracted with methylene chloride. The organic phase was dried and evaporated down, and the oily residue was heated with heptane. The mixture was cooled, the supernatant heptane phase was decanted, and the process was repeated several times. Finally, 0.8 g of the title compound of melting point 126°-127° C. crystallized out from the heptane solution and was filtered off under suction.

Provenance & Evidence