反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
Into a 1-liter pressure reactor was charged a mixture of iodine monochloride (390 g, 2.4 mol) and chlorosulfonic acid (490 g, 4.206 mol). The reactor was cooled and kept at 0-10° C. until 300 g of tetrafluoroethylene (3.0 mol) was added. After the addition of TFE was complete, the reaction mixture was held at 0-10° C. for 6 hr, at 25° C. for 2 hr and at 50° C. for 2 hr. The reaction mixture was then slowly poured into a large amount of ice with stirring, and worked up as described above. The desired product was obtained (610 g, 74% yield), bp. 62-64° C./6.7 kPa. 19F NMR (188.24 MHz, CDCl3): -85.6 (t, J=4.5 Hz, 2F), -65.3 (t, J=4.5 Hz, 2F). Anal. Calcd. for C2F4IClSO3 : C: 7.02, F: 22.19; Found: C: 7.19, F: 22.73.
WORKUP
后处理
- additionInto a 1-liter pressure reactor was charged
- temperatureThe reactor was cooled
- additionwas added
- additionAfter the addition of TFE
- additionThe reaction mixture was then slowly poured into a large amount of ice