Hexafluoropropylene → 1,2-Oxathietane, 3,4,4-trifluoro-3-(trifluoromethyl)-, 2,2-dioxide
반응식
[OH:1][S:2]([OH:5])(=O)=[O:3].O=S(=O)=O.[F:10][C:11]([F:18])([F:17])[C:12]([F:16])=[C:13]([F:15])[F:14]>>[C:12]1([F:16])([C:11]([F:18])([F:17])[F:10])[S:2](=[O:5])(=[O:3])[O:1][C:13]1([F:15])[F:14]참가 물질
3
반응 조건
- 온도
- 43 °C
실험 절차
Using essentially the procedure of Example 1, the reactor was charged with 33.8 g of 67 wt. % oleum (0.28 mole SO3) and 58.0 g hexafluoropropene. After the initial exotherm (max. pressure 896 kPa at 39° C.) the mixture was heated for 13 hours at 43° C. The reactor was vented of excess hexafluoropropene (16.0 g recovered including HFP collected during followed distillation). There was consumed 42.0 g (0.28 mole) HFP. The two phase reaction solution (70.1 g) was distilled using a concentric tube column to yield HFP sultone (39.8 g, 62% yield based on HFP consumed, b.p. 47° C.). The distillation residue was then distilled using a mini-lab apparatus to give 5.4 g of an intermediate fraction with a b.p. of 56°-155° C., 20 g of a fraction with a b.p. of 156°-167° C., and 1.3 g ofundistilled residue. The fraction with b.p. 156°-167° C. was analyzed by 19F and 1H NMR to reveal a complex mixture of primarily fluorosulfonic acid and several acid fluorides, sulfonyl fluorides, and at least three tetrafluoropropionic acid derivatives of the structure CF3CHFCOX, where X=F, OSO2F and possibly OCOCHFCF3. The molar ratio of HSO3F to all CHF compounds was 88:35.