DOI: 10.15227/orgsyn.000.0023
TETRAMETHYLBIPHOSPHINE DISULFIDE
Warning: It has been reported1,2 that serious explosions have occurred during the preparation of tetramethylbiphosphine disulfide by the method described in Inorganic Syntheses.3 No such incidents have been reported in the synthesis of the compound published in this series,
4 but the two procedures are sufficiently similar that caution is indicated. The following precautions are strongly urged:
- The phosphorus trichloride sulfide (PSCl3) should be distilled before use.
- The reaction vessel should be cooled with an ice-salt bath (rather than an acetone dry ice bath as specified in the published procedure) during the addition of the PSCl3 solution to the Grignard reagent. The reaction temperature should be monitored carefully. If it falls below -5°, the addition should be stopped and the reaction mixture cautiously rewarmed to 0-5°C before addition is resumed.
- The reaction apparatus should be shielded throughout the addition of the PSCl solution and the subsequent warming of the reaction mixture.
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