反应 #1755448

ord-795c793a725a428caabec4605298cb05

反应方程式

[K+].[OH-]
potassium hydroxide
OCC(F)(F)C(F)F
2,2,3,3-tetrafluoropropan-1-ol
O=S(=O)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F
1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonyl fluoride
[K+].[OH-]
potassium hydroxide
O=S(=O)(OCC(F)(F)C(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F
2,2,3,3-tetrafluoropropyl 1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonate

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The flask was equipped with a magnetic stirrer, cold water condenser
  2. 2
    其他did not exceed 35° C
  3. 3
    过滤Precipitated salts were then filtered from the mixture
  4. 4
    其他the lower liquid fluorochemical product phase was separated from the upper aqueous phase
  5. 5
    其他were removed from the liquid fluorochemical product phase by atmospheric distillation

实验过程

2,2,3,3-tetrafluoropropan-1-ol (202 g, 1.52 mol, obtained from Sinochem Corp.), 1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonyl fluoride (465 g, 1.52 mol, obtained from 3M Company) and water (500 g) were combined in a 3-liter, 3-necked round bottom flask. The flask was equipped with a magnetic stirrer, cold water condenser, thermocouple and an addition funnel. Aqueous potassium hydroxide (45 percent by weight, 211.5 g, 1.7 mol, obtained from Aldrich Chemical Co., Milwaukee, Wis.) was added dropwise via the addition funnel at such a rate that the temperature did not exceed 35° C. Once the addition of the potassium hydroxide was complete, the mixture was stirred for 16 hours at room temperature. Precipitated salts were then filtered from the mixture and the lower liquid fluorochemical product phase was separated from the upper aqueous phase. Unreacted 2,2,3,3-tetrafluoropropan-1-ol and 1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulfonyl fluoride were removed from the liquid fluorochemical product phase by atmospheric distillation.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07988877B2uspto-grants-2011_08