Cesium fluoride → HCID 59457671, 화합물

Compound 452 (22.36 g, 26.6 mmol), iodide 408 (7.904 g, 19.0 mmol), CsF (8.658 g, 57 mmol), NaHCO3 (4.788 g, 57 mmol) and Pd(PPh3)4 (2.195 g, 1.9 mmol) were combined with a mixture of H2O (25 mL) and DME (100 mL) which was with nitrogen for a half-an-hour and heated to reflux overnight. It was then was cooled to RT, diluted with EtOAc (200 ml), washed with aqueous NaHCO3 (50 mL) and brine (50 mL), and concentrated. The residue was purified by flash column chromatography (eluent pure EtOAc to 5% MeOH/EtOAc) followed by trituration with EtOAc/ether, to produce compound 453 as an off-white solid (5.4 g, 50% yield). LCMS: 565 (M+H)+.

1. waitwas with nitrogen for a half-an-hour
2. temperatureheated
3. temperatureto reflux overnight
4. washwashed with aqueous NaHCO3 (50 mL) and brine (50 mL)
5. concentrationconcentrated
6. customThe residue was purified by flash column chromatography (eluent pure EtOAc to 5% MeOH/EtOAc)

ORD 기록

ord-defc9140296844cdb4df74a730f2b894

출처 데이터셋

uspto-grants-2010_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07790729B2