反応 #1755448

ord-795c793a725a428caabec4605298cb05

反応方程式

[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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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