Silver difluoride, reaction with phenyl

Sebacic acid, 43, 39 Sebacoyl chloride, 43, 37 2,2 -SebacoyldicycIohexanone, 43, 34 Silver difluoride, reaction with phenyl disulfide, 44, 82 Silver monofluoride, 44, 82 Sodium amide, as catalyst for carbona-tion of methylacetylene, 42, 98 for formation of sodium sodiophenyl-acetate, 40, 38... 

A 1-1., four-necked, round-bottomed flask equipped with reflux condenser, sealed stirrer, thermometer, and solid addition funnel and protected from atmospheric moisture with a Drierite guard tube is carefully dried and flushed with a dry inert gas (Note I). The flask is charged with 453 g. (3.1 moles) of silver difluoride (Note 2) and 500 ml. of l,l,2-trichloro-l,2,2-trifluoroethane (Note 3), and phenyl disulfide (100 g., 0.458 mole) (Note 4) is weighed into the solid addition funnel. The stirrer is started, and phenyl disulfide is added to the slurry in small portions. An exothermic reaction occurs, and after the addition of several portions the reaction mixture reaches a temperature of 40° (Note 5). By intermittent use of a cooling bath and by adjusting the rate of addition of the disulfide, the reaction temperature may be maintained between 35° and 40°. The addition of the phenyl disulfide requires 45-60 minutes. On completion of the addition the suspension of black silver difluoride has been converted to yellow silver monofluoride, and the exothermic reaction gradually subsides. The reaction mixture is stirred for an additional 15-30 minutes without external cooling and then quickly heated to reflux. 

---