Methane → HCID 14665031, compound

Participants

Reaction Steps

In a 1 liter VA stainless steel autoclave, 85.1 g (0.24 mol) of 5-(2-chloro-1,1,2-trifluoroethoxy)-2-(4-nitrophenylazo)pyridine were hydrogenated in 600 ml of acetic acid, with addition of 10 g of palladium (10%) on activated charcoal, using 61 bar (take-up) of hydrogen at 20°-25° C. The mixture was filtered and the solvent removed by distillation on a rotary evaporator. The residue was taken up in 500 ml of dichloromethane, washed with 100 ml of 20% strength aqueous sodium carbonate and four times with 100 ml of water in each case, and dried over sodium sulfate. The solvent was subsequently removed by evaporation on a rotary evaporator and the residue was distilled in a high vacuum.

Provenance & Evidence