تفاعل #42130

ord-fa0cd374b0cc4fe19f693b35234da701

معادلة التفاعل

O=S(=O)(O)Cl
chlorosulfuric acid
FC(F)=CC(F)(F)F
1,1,3,3,3-pentafluoropropene
O=S(=O)(Cl)OC(F)(F)CC(F)(F)F
CF3CH2CF2OSO2Cl
المردود 72.7%

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled in liquid nitrogen
  2. 2
    أخرىevacuated
  3. 3
    درجة الحرارةto warm
  4. 4
    workup.WAITAfter 24 hours
  5. 5
    أخرىthe reaction mixture quenched by ice
  6. 6
    غسيلthe organic layer washed with 5% sodium bicarbonate, water
  7. 7
    أخرىdried under MgSO4
  8. 8
    workup.DISTILLATIONAfter distillation

الإجراء التجريبي

A 250 mL Hastelloy shaker tube was loaded with 60 g (0.51 mole) chlorosulfuric acid (HOSO2Cl), cooled in liquid nitrogen, evacuated and loaded with 60 g (0.45 mole) of 1,1,3,3,3-pentafluoropropene. The reaction vessel was allowed to warm and kept on a shaker at 20° C. at autogenous pressure for 24 hours. After 24 hours, the pressure tube was unloaded, and the reaction mixture quenched by ice and the organic layer washed with 5% sodium bicarbonate, water and dried under MgSO4. After distillation, 81.3 g of CF3CH2CF2OSO2Cl was obtained containing 6% of CF3CH2CF2OSO2F.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728183B2uspto-grants-2010_06