HRID1276567

反应详情

EQUATION

反应方程式

HRID 1276567 的结构方程式

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

  1. additionInto a 1-liter pressure reactor was charged
  2. temperatureThe reactor was cooled
  3. additionwas added
  4. additionAfter the addition of TFE
  5. additionThe reaction mixture was then slowly poured into a large amount of ice