Propionitrile → 2-Bromo-4-phenylpyridine

4-Phenyl-pyridine-2-carbaldehyde: To a clear, colorless solution of 1A (0.850 g, 4.5 mmol) in propionitrile (4.5 mmol) was added trimethylsilyl bromide (2.95 mL, 22.4 mmol). The resulting orange suspension was microwaved in a sealed tube at 150° C. for 10 min. The reaction was cooled to rt and poured into 1.0 N NaOH containing ice. The aqueous layer was extracted with diethyl ether (2×). The combined organic layers were washed with sat. NaHCO3, brine, dried over Na2SO4, filtered and concentrated to give 1.07 g of 2-bromo-4-phenyl pyridine as an off-white solid. MS 233.9 (M+H)+ and 235.9 (M+2+H)+.

1. customThe resulting orange suspension was microwaved in a sealed tube at 150° C. for 10 min
2. additioncontaining ice
3. extractionThe aqueous layer was extracted with diethyl ether (2×)
4. washThe combined organic layers were washed with sat. NaHCO3, brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated

ORDレコード

ord-9db78dd831754311a32348aedf68589c

出典データセット

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07429604B2