Water → 5,6-Bis(4-bromophenyl)-2,2'-bipyridine

Temperatur

140 °C

In a 500 mL three-neck flask were put 13 g (27 mmol) of 5,6-bis(4-bromophenyl)-3-(2-pyridyl)-1,2,4-triazine, 9.0 mL (83 mmol) of 2,5-Norbornadiene, and 150 mL of xylene. This mixture was refluxed at 140° C. for 5 hours under a nitrogen stream. After a certain time, water was added to the mixture, and an aqueous layer was extracted with toluene. The extract was washed with a saturated saline together with the organic layer, and the organic layer was then dried with magnesium sulfate. The mixture was subjected to gravity filtration, and the obtained filtrate was concentrated to give a solid. The solid was refined with silica gel column chromatography (toluene), so that a target substance, 7.5 g of light-yellow powder was obtained in a yield of 59%.

1. customIn a 500 mL three-neck flask were put
2. extractionan aqueous layer was extracted with toluene
3. washThe extract was washed with a saturated saline together with the organic layer
4. dry with materialthe organic layer was then dried with magnesium sulfate
5. filtrationThe mixture was subjected to gravity filtration
6. concentrationthe obtained filtrate was concentrated
7. customto give a solid

ORD-Eintrag

ord-b62f033a0c094bbeaaf3c9f1834392e0

Quelldatensatz

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09209408B2