Ammonium Chloride → HCID 86698847, compound

Temperature

23 °C

In a 50 mL round-bottom flask equipped with a reflux condenser is placed 3-(4-bromo-2-methoxyphenyl)-2,2-dichlorocyclobutanone (300 mg, 1.08 mmol) and activated zinc (280 mg, 4.30 mmol), in a saturated methanolic ammonium chloride solution (2 ml), the suspension is refluxed for 6 hr, then cooled to 23° C. and filtered through celite and rinsed with petroleum ether (10 mL), and organics are rinsed with water (10 mL), sat sodium bicarbonate (10 mL) and brine (10 ml), dried over sodium sulfate and concentrated under reduced pressure, the crude material was purified by silica gel chromatography to give the title compound (200 mg, 85%).

1. customIn a 50 mL round-bottom flask equipped with a reflux condenser
2. filtrationfiltered through celite
3. washrinsed with petroleum ether (10 mL)
4. washorganics are rinsed with water (10 mL)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customthe crude material was purified by silica gel chromatography

ORD record

ord-5e1b24b599334ce3b17d68d1aad6f16c

Source dataset

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08889730B2