반응 #344429

ord-51abbd3b9c1d4d3eb42c0a8e87597d6b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    온도the reaction mixture was refluxed for 1 hour
  3. 3
    기타Lower layer was separated
  4. 4
    세척washed with water

실험 절차

To a stirred solution of 1,2-dichloro-1,1,2,3,3,4,4,-heptafluoro-6-iodohexane (370.0 g) and ethanol (400 mL) was added dropwise a solution of potassium hydroxide (56.0 g), ethanol (300 mL) and water (20 mL) at 80°-90° C. over 40 minutes. After the addition was complete, the reaction mixture was refluxed for 1 hour and then poured into water. Lower layer was separated and washed with water to give desired product (233.5 g). 19F NMR: -63.9 (m, 2F), -111.9 (m, 2F), -116.2 (m, 2F), -130.5 (m, 1F); 1H NMR: 5.72 to 6.10 (m). IR: 1651 (m), 1422 (s), 1180 (s), 1055 (s), 1019 (s), 1002 (s), 980 (s).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05260492uspto-grants-1993_11