反应详情

温度

70 °C

Phosphorus pentachloride (79.3 g, 0.381 mole) and sodium (methylsulfonyl)methanesulfonate (Formula II with Y=Na, X=H and R=CH3 ; 70 g, 0.359 mole) were stirred with 150 ml of phosphorus oxychloride. As the mixture was warmed to 70° C. in an oil bath, hydrogen chloride was slowly evolved, and the slurry thinned enough to be stirred with a magnetic stirrer. The mixture was heated for 18 hours in an oil bath at 80°-90° C., cooled, and filtered, and the residue was washed with dry chloroform. The chloroform caused the product to precipitate in the filtrate. The precipitate was collected, washed with a small amount of chloroform, and dried over sodium hydroxide pellets: yield, 28.5 g (41%); mp 109°-111° C.; MS (direct-probe temperature, 20° C.) m/e 193 (M+H), 192 (M), 177 (M-CH3), 157 (CH3SO2CH2SO2), 143, 141, 113 (CH2SO2Cl), 98 (CH3SOCl), 94, 93 (CH3SO2CH2), 79 (CH3SO2), 78, 64, 63 (CH3SO); IR (cm-1, strong and medium bands) 3045, 3025, 2995 s, 2930 s, 1405, 1390 s, 1380 s, 1360, 1335 s, 1325 sh, 1315 s, 1225, 1175 s, 1160 s, 1110 s, 980 s, 965, 860 s, 760 s, 695, 595 s, 515 s, 495 s, 460 s.

1. temperatureThe mixture was heated for 18 hours in an oil bath at 80°-90° C.
2. temperaturecooled
3. filtrationfiltered
4. washthe residue was washed with dry chloroform
5. customto precipitate in the filtrate
6. customThe precipitate was collected
7. washwashed with a small amount of chloroform
8. dry with materialdried over sodium hydroxide pellets
9. customyield
10. customIR (cm-1, strong and medium bands) 3045, 3025, 2995 s, 2930 s, 1405, 1390 s, 1380 s, 1360, 1335 s, 1325 sh, 1315 s, 1225, 1175 s, 1160 s, 1110 s, 980 s, 965, 860 s, 760 s, 695, 595 s, 515 s, 495 s, 460 s