Cesium carbonate → HCID 86614996, Verbindung

Dissolve 2,6-dichloro-isonicotinic methyl ester (2.0 g, 10 mmol), palladium (II) acetate (224.0 mg, 1.0 mmol), racemic 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (632 mg, 1.0 mmol) and cesium carbonate (3.96 g, 12 mmol) in toluene (20 mL) in a previously degassed sealed vessel. Flush the mixture with nitrogen gas. Add (S)-(+)-sec-butylamine (1.2 mL, 12 mmol) to the solution and heat the sealed mixture overnight at 100° C. Cool to room temperature and dilute with diethyl ether and filter through a filtering agent. Concentrate the filtrate and purify (silica gel chromatography, eluting with 0:100 to 10:90 ethyl acetate:hexanes) to give the title compound (73%).

1. customa previously degassed
2. customsealed vessel
3. customFlush the mixture with nitrogen gas
4. filtrationfilter through a filtering agent
5. concentrationConcentrate the filtrate
6. custompurify
7. wash(silica gel chromatography, eluting with 0:100 to 10:90 ethyl acetate:hexanes)

ORD-Eintrag

ord-2816ef09826a4ce483e8a069bfb3ac49

Quelldatensatz

uspto-grants-2009_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07618978B2