Réaction #554598

ord-b2224c9c4deb4cde88f2e91f24b2fb9e

Équation de réaction

COc1cccc(-c2ccccc2-c2ccccc2)c1
3-methoxy[1,1′:2′,1″]terphenyl
COc1ccc2c3ccccc3c3ccccc3c2c1
2-methoxytriphenylene
Rendement 60.0%

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    FiltrationThe reaction solution was subjected to filtration
  2. 2
    Lavageby washing with an excessive amount of acetone
  3. 3
    workup.DISSOLUTIONThe resulting solid was dissolved in heated toluene
  4. 4
    FiltrationInsoluble substances were filtered out
  5. 5
    Autrefollowed by crystallization
  6. 6
    Températurewith cooling
  7. 7
    FiltrationThe resulting crystal was collected by filtration

Mode opératoire

23.4 g of 3-methoxy[1,1′:2′,1″]terphenyl, 146 g of iron (III) chloride and 200 mL of methylene chloride were placed in a flask, and stirred for one hour while deaerating with argon. The reaction solution was subjected to filtration, followed by washing with an excessive amount of acetone. The resulting solid was dissolved in heated toluene. Insoluble substances were filtered out, followed by crystallization with cooling. The resulting crystal was collected by filtration to obtain 13.9 g (yield: 60%) of 2-methoxytriphenylene.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08623520B2uspto-grants-2014_01