2,5-Dihydrofuran → N-(4-(3-(2,3-Dihydrofuran-2-YL)pyridin-2-yloxy)phenyl)pyridin-2-amine

온도

80 °C

To a 25 mL microwave vial was added Bis(tri-tert-butylphosphine) palladium (0) (121 mg, 0.238 mmol) and N-(4-(3-bromopyridin-2-yloxy)phenyl)pyridin-2-amine hydrochloride (900 mg, 2.377 mmol) before sealing and evacuating and backfilling with nitrogen (2×). After addition of dioxane (11.900 ml), N-cyclohexyl-N-methylcyclohexanamine (1.008 ml, 4.75 mmol), and 2,5-dihydrofuran (0.701 ml, 9.51 mmol), the black suspension was heated to 80° C. for 5 h. The reaction mixture was cooled to room temperature, transferred to a 100 mL round bottom flask, and concentrated under reduced pressure. The material was taken up in DCM and adsorbed onto silica before purifying by flash chromatography (0 to 75% ethyl acetate/hexanes), affording a mixture of 2- and 3-dihydrofuranyl products that was used in subsequent reactions.

1. customevacuating
2. temperatureThe reaction mixture was cooled to room temperature
3. customtransferred to a 100 mL round bottom flask
4. concentrationconcentrated under reduced pressure
5. custombefore purifying by flash chromatography (0 to 75% ethyl acetate/hexanes)
6. customaffording

ORD 기록

ord-705209111c234a03a4925a7d528962ba

출처 데이터셋

uspto-grants-2014_01

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08637500B2