Nitrogen → HCID 67392089, Verbindung

Temperatur

0 °C

100 ml abs. tetrahydrofurane (THF) are cooled to 0° C. in an inert gas atmosphere (N2) and mixed with 2.00 g (10.9 mmol) of 4,4′-dimethyl-2,2′-bipyridine. After stirring for 15 min at 0° C. 5.45 ml (10.9 mmol) of a 2 M solution of lithium diisopropylamide (LDA) are added to the THF which is then reacted for 2 hr with cooling. The reaction solution is added dropwise over a period of 30 min to a solution of 3.30 g (11.0 mmol) of 1.10 dibromodecane in 30 ml abs. THF at 0° C. The brownish clear solution is stirred for a further 2 hr at 0° C. and for 16 hr at RT before being quenched with 10 ml H2O. The suspension is then concentrated under a reduced pressure almost until dry. The aqueous residue is taken up in 25 ml of water, and 25 ml brine is added and the mixture extracted three times with 75 ml CHCl3 each. The organic phases are dried over Na2SO4, filtered and concentrated until dry under a reduced pressure. Purifying of the product mixture is achieved on silica gel with ethyl acetate (EtOAc). The product A is obtained in the form of a beige crystalline powder.

1. customis then reacted for 2 hr
2. temperaturewith cooling
3. customat 0° C
4. stirringThe brownish clear solution is stirred for a further 2 hr at 0° C. and for 16 hr at RT
5. custombefore being quenched with 10 ml H2O
6. concentrationThe suspension is then concentrated under a reduced pressure almost
7. customuntil dry
8. addition25 ml brine is added
9. extractionthe mixture extracted three times with 75 ml CHCl3 each
10. dry with materialThe organic phases are dried over Na2SO4
11. filtrationfiltered
12. concentrationconcentrated
13. customuntil dry under a reduced pressure
14. customPurifying of the product mixture

ORD-Eintrag

ord-14cb40ee9f5e4798b1f2752c49fcc72f

Quelldatensatz

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08883671B2