Triethylamine → 6-Di-iso-propylphosphinomethyl-2,2'-bipyridine

Temperatur

50 °C

stirring bar was added 6-chloromethyl-2,2′-bipyridine (BPy-CH2Cl) (1.03 g, 5.00 mmol), di-iso-propyl phosphine (710 mg, 6.00 mmol), and 15 mL MeOH in nitrogen glove box. The flask was sealed and heated at 50° C. for 48 hrs with stirring outside the glove box. After cooling, it was reintroduced to the glove box, triethylamine (910 mg, 9.00 mmol) was added and the reaction mixture was stirred at room temperature for 1 hr. The solvents were removed under reduced pressure to obtain a white solid. The residue was washed with ether (2×10 mL), filtered and was removed under reduced pressure to yield a pale yellow liquid. It was further purified by basic alumina chromatography under the glove box using hexane as an eluent to yield pure 6.

1. customThe flask was sealed
2. stirringwith stirring outside the glove box
3. temperatureAfter cooling
4. additionwas added
5. stirringthe reaction mixture was stirred at room temperature for 1 hr
6. customThe solvents were removed under reduced pressure
7. customto obtain a white solid
8. washThe residue was washed with ether (2×10 mL)
9. filtrationfiltered
10. customwas removed under reduced pressure
11. customto yield a pale yellow liquid
12. customIt was further purified by basic alumina chromatography under the glove box
13. customto yield pure 6

ORD-Eintrag

ord-adc6445ae5d347ddb61cc7e1793e658f

Quelldatensatz

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09045381B2