Réaction #1458418

ord-e46395004e664909bfd2812dc56a087b

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONwas added
  2. 2
    workup.DISSOLUTIONto dissolve the same
  3. 3
    workup.STIRRINGstirred for 1 hour
  4. 4
    TempératureThe mixture was cooled again to −90° C.
  5. 5
    TempératureAfter warming
  6. 6
    Autreto react
  7. 7
    Températureunder reflux for 12 hours

Mode opératoire

2.0 g of 4,4′-dibromo-2,2′-diiodo-5,5′-dioctyloxy-1,1′-biphenyl synthesized as above was put in a 100 ml flask in an atmosphere of nitrogen and 20 ml of tetrahydrofuran was added to dissolve the same. Then, the tetrahydrofuran solution was cooled to −90° C. and 3.4 ml of 1.6M hexane solution was added dropwise. After 1-hour stirring, a solution of 1.5 g of magnesium bromide in 20 ml of tetrahydrofuran was added, warmed to room temperature, and stirred for 1 hour. The mixture was cooled again to −90° C., and 1.01 g of (2,4,6-triisopropylphenyl)dimethoxyborane was added. After warming, the mixture was allowed to react under reflux for 12 hours.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07157154B2uspto-grants-2007_01