تفاعل #1755448

ord-795c793a725a428caabec4605298cb05

معادلة التفاعل

[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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07988877B2uspto-grants-2011_08